1,2-Dichloroethane → Tert-butyl{2-[[(7r)-11-({[(3-chloropropyl)sulfonyl]amino}carbonyl)-14-cyclohexyl-7,8-dihydro-6h-indolo[1,2-e][1,5]benzoxazocin-7-yl](methyl)amino]ethyl}carbamate

HRID 421932

反応式

[Cl:1][CH2:2][CH2:3][CH2:4][S:5]([NH2:8])(=[O:7])=[O:6].C(Cl)CCl.[C:13]([O:17][C:18]([NH:20][CH2:21][CH2:22][N:23]([CH3:52])[C@@H:24]1[CH2:31][N:30]2[C:32]3[CH:33]=[C:34]([C:45](O)=[O:46])[CH:35]=[CH:36][C:37]=3[C:38]([CH:39]3[CH2:44][CH2:43][CH2:42][CH2:41][CH2:40]3)=[C:29]2[C:28]2[CH:48]=[CH:49][CH:50]=[CH:51][C:27]=2[O:26][CH2:25]1)=[O:19])([CH3:16])([CH3:15])[CH3:14]>CN(C1C=CN=CC=1)C.C(Cl)Cl>[C:13]([O:17][C:18](=[O:19])[NH:20][CH2:21][CH2:22][N:23]([C@@H:24]1[CH2:31][N:30]2[C:32]3[CH:33]=[C:34]([C:45]([NH:8][S:5]([CH2:4][CH2:3][CH2:2][Cl:1])(=[O:7])=[O:6])=[O:46])[CH:35]=[CH:36][C:37]=3[C:38]([CH:39]3[CH2:44][CH2:43][CH2:42][CH2:41][CH2:40]3)=[C:29]2[C:28]2[CH:48]=[CH:49][CH:50]=[CH:51][C:27]=2[O:26][CH2:25]1)[CH3:52])([CH3:16])([CH3:14])[CH3:15]

参加物

反応条件

温度: 40 °C

実験手順

3-chloropropane-1-sulfonamide (1.8 eq), DMAP (2.9 eq) and EDC (1.8 eq), were added to a solution of (7R)-7-[{2-[(tert-butoxycarbonyl)amino]ethyl}(methyl)amino]-14-cyclohexyl-7,8-dihydro-6H-indolo[1,2-e][1,5]benzoxazocine-11-carboxylic acid (prepared as described in Example 1, Step 7) (0.025 M) in DCM. The reaction was stirred under N2 at 40° C. for 2 h, before being allowed to cool. Volatiles were removed in vacuo to leave the crude product as a yellow gum which could be taken on without further purification. (ES+) m/z 687 (M+H)+; 689 (M+H)+

後処理

temperatureto cool
customVolatiles were removed in vacuo

出典と根拠

ORDレコード: ord-dd02d376464e4968b8a6dd21f3bd5c29
出典データセット: uspto-grants-2012_01
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08101595B2

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 2

反応条件

実験手順

後処理

出典と根拠

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