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 1669435ノート

反応式

HRID 1669435 の反応式
[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

参加物

7

反応物 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

生成物 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

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
40 °C

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-4d6c85750a014324b48f4aa8c3d21414
出典データセット
uspto-grants-2011_08
特許番号
US07989438B2

反応ノート

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