1,2-Dichloroethane → Tert-butyl (2-{13-cyclohexyl-10-[({[(2,2-dimethoxyethyl)(methyl)amino]sulfonyl}amino)carbonyl]-3-methoxy-6,7-dihydro-5H-indolo[2,1-a][2]benzazepin-6-yl}ethyl)methylcarbamate

HRID 1669435노트

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HRID 1669435 반응식
[C:1]([O:5][C:6]([N:8]([CH3:40])[CH2:9][CH2:10][CH:11]1[CH2:17][C:16]2[CH:18]=[C:19]([O:22][CH3:23])[CH:20]=[CH:21][C:15]=2[C:14]2=[C:24]([CH:34]3[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]3)[C:25]3[CH:26]=[CH:27][C:28]([C:31](O)=[O:32])=[CH:29][C:30]=3[N:13]2[CH2:12]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:41][O:42][CH:43]([O:51][CH3:52])[CH2:44][N:45]([CH3:50])[S:46]([NH2:49])(=[O:48])=[O:47].C(Cl)CCl>C(Cl)Cl.CN(C1C=CN=CC=1)C.CCOC(C)=O>[CH:34]1([C:24]2[C:25]3[CH:26]=[CH:27][C:28]([C:31]([NH:49][S:46]([N:45]([CH2:44][CH:43]([O:42][CH3:41])[O:51][CH3:52])[CH3:50])(=[O:48])=[O:47])=[O:32])=[CH:29][C:30]=3[N:13]3[CH2:12][CH:11]([CH2:10][CH2:9][N:8]([CH3:40])[C:6](=[O:7])[O:5][C:1]([CH3:3])([CH3:2])[CH3:4])[CH2:17][C:16]4[CH:18]=[C:19]([O:22][CH3:23])[CH:20]=[CH:21][C:15]=4[C:14]=23)[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1

참가 물질

7

반응물 3

HCID 111,2-DichloroethaneHCID 673450216-{2-[(tert-butoxycarbonyl)(methyl)amino]ethyl}-13-cyclohexyl-3-methoxy-6,7-dihydro-5H-indolo[2,1-a][2]benzazepine-10-carboxylic acidHCID 86627889N-(2,2-dimethoxyethyl)-N-methylsulfamide

생성물 1

HCID 67342477Tert-butyl (2-{13-cyclohexyl-10-[({[(2,2-dimethoxyethyl)(methyl)amino]sulfonyl}amino)carbonyl]-3-methoxy-6,7-dihydro-5H-indolo[2,1-a][2]benzazepin-6-yl}ethyl)methylcarbamate

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

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온도
40 °C

실험 절차

To a solution of 6-{2-[(tert-butoxycarbonyl)(methyl)amino]ethyl}-13-cyclohexyl-3-methoxy-6,7-dihydro-5H-indolo[2,1-a][2]benzazepine-10-carboxylic acid in DCM (0.07M), N-(2,2-dimethoxyethyl)-N-methylsulfamide (2 eq, Example 1, Step 1), EDC (3 eq) and DMAP (5 eq) were added. The mixture was stirred at 40° C. for 3 h, then diluted with EtOAc and washed with 1N HCl, 1N NaOH solution and brine. The organic phase was dried over Na2SO4 and evaporated in vacuo and the residual material was used in the next step without purification. (ES+) m/z 727 (M+H)+.

후처리

  1. washwashed with 1N HCl, 1N NaOH solution and brine
  2. dry with materialThe organic phase was dried over Na2SO4
  3. customevaporated in vacuo
  4. customthe residual material was used in the next step without purification

출처 및 근거

ORD 기록
ord-4d6c85750a014324b48f4aa8c3d21414
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989438B2

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