HRID1849257

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID313

Hydrochloric Acid

ClH

结构：CN(C(=O)c1cc2c(s1)-c1ccc(C(=O)NCCS(C)(=O)=O)cc1OCC2)c1cc(C(=O)N2CCN(C(=O)OC(C)(C)C)CC2)ccc1Cl

HCID58204219

未命名化合物

PRODUCTS

生成物

结构：CN(C(=O)c1cc2c(s1)-c1ccc(C(=O)NCCS(C)(=O)=O)cc1OCC2)c1cc(C(=O)N2CCNCC2)ccc1Cl

HCID58203814

未命名化合物

收率 58.3%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID8857

Ethyl acetate

C4H8O2

2 次

PROCEDURE

实验过程

A solution of HCl in EtOAc (4M, 20 mL) was slowly added into a solution of tert-butyl 4-(4-chloro-3-(N-methyl-8-(2-(methylsulfonyl)ethylcarbamoyl)-4,5-dihydrobenzo[b]thieno[2,3-d]oxepine-2-carboxamido)benzoyl)piperazine-1-carboxylate (350 mg, 0.48 mmol) in EtOAc (5 mL) at 0° C. The mixture was stirred at room temperature for overnight. The solids were filtered and washed with EtOAc, dried to give 334 (176.6 mg, yield: 55%). 1H NMR (MeOD, 400 MHz): δ7.77-7.44 (m, 7H, ArH, NH), 6.93 (s, 1H, ═CH), 4.24-3.04 (m, 23H). LC-MS: (ESI, m/z)=631 [M+H]+

WORKUP

后处理

filtrationThe solids were filtered
washwashed with EtOAc
customdried

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-71f56b961b434ae7ba8cc99ff50ab944
来源数据集: uspto-grants-2015_02
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08952043B2
来源说明: uspto-grants-2015_02

反应 SMILES

Cl.[Cl:2][C:3]1[CH:23]=[CH:22][C:6]([C:7]([N:9]2[CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][CH2:10]2)=[O:8])=[CH:5][C:4]=1[N:24]([CH3:50])[C:25]([C:27]1[S:49][C:30]2[C:31]3[CH:39]=[CH:38][C:37]([C:40](=[O:48])[NH:41][CH2:42][CH2:43][S:44]([CH3:47])(=[O:46])=[O:45])=[CH:36][C:32]=3[O:33][CH2:34][CH2:35][C:29]=2[CH:28]=1)=[O:26]>CCOC(C)=O>[Cl:2][C:3]1[CH:23]=[CH:22][C:6]([C:7]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[O:8])=[CH:5][C:4]=1[N:24]([CH3:50])[C:25]([C:27]1[S:49][C:30]2[C:31]3[CH:39]=[CH:38][C:37]([C:40]([NH:41][CH2:42][CH2:43][S:44]([CH3:47])(=[O:45])=[O:46])=[O:48])=[CH:36][C:32]=3[O:33][CH2:34][CH2:35][C:29]=2[CH:28]=1)=[O:26]