HRID80577

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID521998

4-Methylbenzenesulfonic acid hydrate

C7H10O4S

结构：CCC[C@@H](NC(=O)N1CC(=NOCC)NC[C@H](Cc2cc(Cl)ccc2OC)C1=O)c1ccc(C(=O)O)c(N)c1

HCID178448362

未命名化合物

PRODUCTS

生成物

结构：CCC[C@@H](NC(=O)N1CC(=NOCC)NC[C@H](Cc2cc(Cl)ccc2OC)C1=O)c1ccc(C(=O)O)c(N)c1.CCC[C@@H](NC(=O)N1CC(=NOCC)NC[C@H](Cc2cc(Cl)ccc2OC)C1=O)c1ccc(C(=O)O)c(N)c1.Cc1ccc(S(=O)(=O)O)cc1.Cc1ccc(S(=O)(=O)O)cc1.Cc1ccc(S(=O)(=O)O)cc1

HCID178448363

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID6342

Acetonitrile

C2H3N

2 次

PROCEDURE

实验过程

The compound 12 obtained at Step (2) (503 mg) was dissolved in acetonitrile (0.5 ml), p-toluenesulfonic acid monohydrate in an acetonitrile solution (0.69M, 2 ml) was added at 60° C., then the mixture was allowed to gradually cool to room temperature. After 3 hours, the mixture was cooled to 0° C. and further stirred for 1.5 hours, then the precipitates were collected by filtration to obtain the title compound (535 mg) as a colorless crystals.

WORKUP

后处理

temperaturethe mixture was cooled to 0° C.
filtrationthe precipitates were collected by filtration

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-8654c9004bf5476abf41d465b9644743
来源数据集: uspto-grants-2014_09
DOI: 10.6084/m9.figshare.5104873.v1
专利: US08846660B2
来源说明: uspto-grants-2014_09

反应 SMILES

[NH2:1][C:2]1[CH:10]=[C:9]([C@H:11]([NH:15][C:16]([N:18]2[C:24](=[O:25])[C@@H:23]([CH2:26][C:27]3[CH:32]=[C:31]([Cl:33])[CH:30]=[CH:29][C:28]=3[O:34][CH3:35])[CH2:22][NH:21][C:20](=[N:36][O:37][CH2:38][CH3:39])[CH2:19]2)=[O:17])[CH2:12][CH2:13][CH3:14])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].O.[C:41]1([CH3:51])[CH:46]=[CH:45][C:44]([S:47]([OH:50])(=[O:49])=[O:48])=[CH:43][CH:42]=1>C(#N)C>[S:47]([C:44]1[CH:45]=[CH:46][C:41]([CH3:51])=[CH:42][CH:43]=1)([OH:50])(=[O:49])=[O:48].[NH2:1][C:2]1[CH:10]=[C:9]([C@H:11]([NH:15][C:16]([N:18]2[C:24](=[O:25])[C@@H:23]([CH2:26][C:27]3[CH:32]=[C:31]([Cl:33])[CH:30]=[CH:29][C:28]=3[O:34][CH3:35])[CH2:22][NH:21][C:20](=[N:36][O:37][CH2:38][CH3:39])[CH2:19]2)=[O:17])[CH2:12][CH2:13][CH3:14])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[S:47]([C:44]1[CH:45]=[CH:46][C:41]([CH3:51])=[CH:42][CH:43]=1)([OH:50])(=[O:49])=[O:48].[S:47]([C:44]1[CH:45]=[CH:46][C:41]([CH3:51])=[CH:42][CH:43]=1)([OH:50])(=[O:49])=[O:48].[NH2:1][C:2]1[CH:10]=[C:9]([C@H:11]([NH:15][C:16]([N:18]2[C:24](=[O:25])[C@@H:23]([CH2:26][C:27]3[CH:32]=[C:31]([Cl:33])[CH:30]=[CH:29][C:28]=3[O:34][CH3:35])[CH2:22][NH:21][C:20](=[N:36][O:37][CH2:38][CH3:39])[CH2:19]2)=[O:17])[CH2:12][CH2:13][CH3:14])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5]