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D-酒石酸單酯單酰胺類化合物的制作方法_2

文檔序號(hào):9465518閱讀:來源:國知局
(1H, d, OCH), 6. 04 (1H, d, OCH), 7. 26 (1H ,t, ArH), 7. 29 (2H, d, ArH), 7. 33 (2H, t, ArH), 8. 45 (H, s, NH). HR-MS: Calcd for C13H17NO5 267. 28, found 267. l〇
[0059] I-10:D_酒石酸單苯酯單酰乙胺
[0060] IH-NMR (400MHz, CDCl3) δ : I. 18 (3H, t, CH3),3· 16 (2H, q, NCH2),3· 20 (1H, brs, OH), 3. 31 (1Η, brs, OH), 5. 79 (1H, d, OCH), 5. 96 (1H, d, OCH), 7. 35 (1H, t, ArH), 7. 42 (2H, d, ArH), 7 ? 49 (2H, t, ArH),8· 31 (H, s, NH) · HR-MS:Calcd for C12H15NO5 253. 25, found 253. I。
[0061] I-Il: D-酒石酸單丁酯單酰乙胺
[0062] lH-NMR(400MHz,CDCl3) δ : 1. 02 (3H,t,CH3),1. 12 (3H,t,CH3),1. 45 (2H,m,CH2),1. 6 2 (2H, m, CH2), 3. 35 (2H, brs, OH), 3, 49 (2H, q, NCH2), 4. 17 (2H, t, OCH2), 5. 71 (1H, d, OCH), 6. 0 9(1H, d, OCH), 8.70(lH,s,NH). HR-MS:Calcd for C10H19NO5 233. 26, found 233. 2〇
[0063] I-12:D_酒石酸單環(huán)己酯單酰乙胺
[0064] 1H-NMR (400MHz, CDCl3) δ : I. 02 (3H, t, CH3),I. 47 (2H, m, CH2),I. 58 (4H, m, CH2),I. 6 0 (4Η, m, CH2), 3. 19 (2Η, q, NCH3), 3. 25 (1Η, brs, OH), 3. 33 (1Η, brs, OH), 3. 98 (1Η, m, OCH), 5. 8 1 (1Η, d, 0CH), 6. 01 (1Η, d, 0CH), 8. 13 (1Η, s, NH). HR-MS:Calcd for C12H21NO5 259. 30, found 259. 2。
[0065] I-13:D-酒石酸單芐酯單酰丙胺
[0066] IH-NMR (400MHz, CDCl3) δ : 〇· 94 (3H, t, CH3),1. 41 (2H, q, CH2),3. 20 (1H, brs, 0H), 3. 37 (1H, brs, OH), 3. 66 (2Η, q, NCH2), 5. 13 (2Η, s, OCH2), 5. 89 (1Η, d, 0CH), 6. 01 (1Η, d, OCH ),7. 29 (1Η, t, ArH), 7. 34 (2Η, d, ArH), 7. 40 (2Η, t, ArH) ,8.15 (Η, s, NH). HR-MS: Calcd for C14H19NO5 281. 30, found 281.2。
[0067] 1-14: D-酒石酸單苯酯單酰丙胺
[0068] IH-匪R (400MHz,CDCl3) δ : 1. 08 (3H,t,CH3), 1. 34 (2H,q,CH2), 3. 21 (1H,brs, 0 Η), 3. 39 (1Η, brs, 0Η), 3. 66 (2Η, q, NCH2), 5. 78 (1Η, d, 0CH), 5. 98 (1Η, d, 0CH), 7. 25 (1Η, t, ArH), 7. 32 (2Η, d, ArH) ,7.41 (2Η, t, ArH), 8. 10 (Η, s, NH). HR-MS: Calcd for C13H17NO5 267. 28, found 267. 2〇
[0069] I-15:D_酒石酸單丁酯單酰丙胺
[0070] 1H-NmrUOOMHz, CDCl3) δ : 1. 02 (3H, t, CH3), 1. 12 (3H, t, CH3), 1. 36 (2H, m, CH2 ),1. 45 (2H, m, CH2), 1. 62 (2H, m, CH2), 3. 26 (2H, brs, 0H), 3, 49 (2H, q, NCH2), 4. 17 (2H, t, OCH2), 5. 71 (1H, d, 0CH), 6. 09 (1H, d, 0CH), 8. 70 (1H, s, NH). HR-MS: Calcd for C11H21NO5 247. 29, found 247. 2。
[0071] 1-16: D-酒石酸單環(huán)己酯單酰丙胺
[0072] 1H-NmrGOOMHz, CDCl3) δ : 1. 01 (3H,t,CH3),1. 43-1. 60 (8H,m,CH2),1. 76 (4H,m,CH2 ),3. 23 (1H, brs, OH), 3. 26 (1H, brs, OH), 3, 51 (2H, q, NCH2), 4. 37 (1H, m, OCH), 5. 71 (1H, d, OC H), 6. 09 (1H, d, OCH), 8. 20 (1H, s, NH). HR-MS: Calcd for C13H23NO5 273. 33, found 273. 2〇
[0073] I-17:D_酒石酸單芐酯單酰異丙胺
[0074] 4-匪1?(4001泡,〇0(:13)5:1.〇4(6!1,(1,01 3),3.21(1!1,1^8,0!〇,3.30(1!1,1^8, OH), 3. 81 (1H, m, NCH), 4. 96 (2H, s, OCH2), 5. 88 (1H, d, OCH), 6. 04 (1H, d, OCH), 7. 26 (1H, t, ArH), 7. 29 (2H, d, ArH), 7. 33 (2H, t, ArH), 8. 45 (H, s, NH). HR-MS: Calcd for C14H19NO5 281. 30, found 281. 2。
[0075] 1-18: D-酒石酸單苯酯單酰異丙胺
[0076] 1H-NMR (400MHz,CDCl3) δ : 1. 18 (6H,d,CH3),3. 22 (1H,brs, 0H),3. 36 (1H,brs, 0H), 3. 66 (2H, q, NCH2), 5. 79 (1H, d, OCH), 5. 96 (1H, d, OCH), 7. 35 (1H, t, ArH), 7. 42 (2H, d, ArH), 7 ,49(2H, t,ArH),8. 31(H, s, NH).HR-MS:Calcd for C13H17NO5 267. 28, found 267. 2〇
[0077] 1-19: D-酒石酸單丁酯單酰異丙胺
[0078] 1H-NmrGOOMHz, CDCl3) δ :〇· 97 (3H, t, CH3),I. 12 (6H, d, CH3),I. 46 (2H, m, CH2),I. 6 4 (2H, m, CH2), 3. 23 (2H, brs, OH), 3, 87 (1H, m, NCH), 4. 20 (2H, t, OCH2), 5. 76 (1H, d, OCH), 6. 11 (1H, d, OCH), 8. 20 (1H, s, NH). HR-MS: Calcd for C11H21NO5 247. 29, found 247. 2〇
[0079] I-20:D_酒石酸單環(huán)己酯單酰異丙胺
[0080] 1H-NMR (400MHz, CDCl3) δ : I. 05 (6H, d, CH3), I. 47 (2H, m, CH2), I. 58 (4H, m, CH2), I. 6 0 (4Η, m, CH2), 3. 33 (2Η, brs, OH), 3. 89 (1Η, m, NCH), 4. 08 (1Η, m, 0CH), 5. 81 (1Η, d, 0CH), 6. 01 (1Η, d, 0CH), 8. 13 (1Η, s, NH). HR-MS:Calcd for C13H23NO5 273. 33, found 273. 3〇
[0081] 1-21 :D_酒石酸單芐酯單酰丁胺
[0082] 1H-匪R (400MHz, CDCl3) δ : 1. 04 (3H, t, CH3),1. 32 (2H, m, CH2),1. 45 (2H, m, CH2),3 .24 (1H, brs, 0H), 3. 29 (1Η, brs, OH), 3. 37 (2H, t, NCH2), 4. 93 (2Η, s, OCH2), 5. 88 (1Η, d, OCH ),6. 04 (1Η, d, 0CH), 7. 26 (1Η, t, ArH), 7. 29 (2Η, d, ArH), 7. 33 (2Η, t, ArH), 8. 25 (Η, s, ΝΗ). HR-MS:Calcd for C15H21NO5 296. 33, found 297. 3〇
[0083] 1-22: D-酒石酸單苯酯單丁酰胺
[0084] 4-匪1?(40010^,0)(:13)5:1.12(3!1,釔01 3),1.33(2!1,111,012),1.56(2!1,111,012),3 .26 (1Η, brs, 0H), 3. 36 (1H, brs, 0H), 3. 76 (2H, t, NCH2), 5. 83 (1H, d, 0CH), 5. 92 (1H, d, OCH ),7. 35 (1H, t, ArH), 7. 42 (2H, d, ArH), 7. 50 (2H, t, ArH), 8. 31 (H, s, NH). HR-MS: Calcd for C14H19NO5 281. 30, found 281.2。
[0085] I-23:D_酒石酸單丁酯單酰丁胺
[0086] 1H-匪R (400MHz,CDCl3) δ : 〇· 97-1. 02 (6H,m,CH3),1. 29 (2H,m,CH2),1. 45 (2H,m, CH2), I. 57 (2H, m, CH2), I. 62 (2Η, m, CH2), 3. 27 (2Η, brs, 0Η), 3, 49 (2Η, t, NCH2), 4. 28 (2Η, t ,OCH2), 5. 71 (1Η, d, 0CH), 6. 09 (1Η, d, 0CH), 7. 90 (1Η, s, NH). HR-MS:Calcd for C12H23NO5 261. 31, found 262. 3〇
[0087] I-24:D_酒石酸單環(huán)己酯單酰丁胺
[0088] 1H-NMR (400MHz, CDCl3) δ : L 15 (3H, t, CH3),1. 29 (2H, m, CH2),1. 37 (2H, m, CH2),1. 5 8 (4H, m, CH2) ,1-60 (4H, m, CH2), 3. 28 (2H, brd, 0H), 3. 29 (2Η, t, NCH2), 4. 28 (1Η, m, OCH), 5. 81 (1H, d, OCH), 6. 08 (1H, d, OCH), 8. 23 (1H, s, NH). HR-MS: Calcd for C14H25NO5 287. 35, found 287. 3〇
[0089] I-25:D_酒石酸單芐酯單酰叔丁胺
[0090] 1H-NmrGOOMHz, CDCl3) δ : I. 34 (9H, s, CH3),3· 22 (1H, brs, OH),3· 31 (1H, brs, OH), 5. 23 (2H, s, OCH2), 5. 88 (1H, d, OCH), 6. 12 (1H, d, OCH), 7. 36 (1H, t, ArH), 7. 41 (2H, d, ArH), 7 ,46(2H, t,ArH),8. 25(H, s, NH).HR-MS:Calcd for C15H21NO5 295. 33, found 295. 3〇
[0091] I-26:D_酒石酸單苯酯單酰叔丁胺
[0092] 1H-NMR (400MHz, CDCl3) δ : I. 35 (9H, s, CH3),3· 23 (1H, brs, OH),3· 34 (1H, brs, OH), 5. 68 (1Η, d, OCH), 5. 89 (1Η, d, OCH), 7. 25 (1Η, t, ArH), 7. 32 (2Η, d, ArH), 7. 39 (2Η, t, ArH), 8. 10 (Η, s,NH).HR-MS:Calcd for C14H19NO5 281. 30, found 281. 2〇
[0093] I-27:D_酒石酸單丁酯單酰叔丁胺
[0094] 1H-NMR (400MHz,CDCl3) δ : 〇· 94 (3H,t,CH3),1. 38 (9H,s,CH3),1. 45 (2H,m,CH2),1. 6 3 (2H, m, CH2), 3. 23 (2H, brs, OH), 4. 17 (2H, t, OCH2), 5. 91 (1H, d, OCH), 6. 14 (1H, d, OCH), 8. 3 9 (lH,s,NH). HR-MS: Calcd for C12H23NO5 261. 31, found 261. 2〇
[0095] I-28:D-酒石酸單環(huán)己酯單酰叔丁胺
[0096] 1H-NMR (400MHz,CDCl3) δ : I. 36 (9H,s,CH3),I. 45 (2H,m,CH2),I. 59 (4H,m,CH2),I. 6 2 (4H, m
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