HRID1790269

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID313

Hydrochloric Acid

ClH

HCID521874

O-Methylhydroxylamine hydrochloride

CH6ClNO

结构：CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=O)c4cccc(Cl)c4)ccc32)cc1

HCID22041531

未命名化合物

PRODUCTS

生成物

结构：CCOC(=O)C(C)(C)Oc1ccc(OCCn2c(=O)sc3cc(C(=NOC)c4cccc(Cl)c4)ccc32)cc1

HCID86760134

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID1049

Pyridine

C5H5N

PROCEDURE

实验过程

A solution of the compound obtained in Step A (1.00 g) and O-methylhydroxylamine hydrochloride (309 mg) in 15 ml of pyridine is heated at reflux for 3 hours. The reaction mixture is hydrolysed using 100 ml of ice-cold water and acidified using 6N HCl. The precipitate obtained is filtered off, washed with water and then recrystallised from petroleum ether by cooling in a freezer to yield the title compound in the form of a white powder.

WORKUP

后处理

temperatureat reflux for 3 hours
customThe precipitate obtained
filtrationis filtered off
washwashed with water
customrecrystallised from petroleum ether
temperatureby cooling in a freezer

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-43e233c2fe6e4d73b14262eec7767f6c
来源数据集: uspto-grants-2006_07
DOI: 10.6084/m9.figshare.5104873.v1
专利: US07071221B2
来源说明: uspto-grants-2006_07

反应 SMILES

[Cl:1][C:2]1[CH:3]=[C:4]([CH:35]=[CH:36][CH:37]=1)[C:5]([C:7]1[CH:34]=[CH:33][C:10]2[N:11]([CH2:15][CH2:16][O:17][C:18]3[CH:32]=[CH:31][C:21]([O:22][C:23]([CH3:30])([CH3:29])[C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:20][CH:19]=3)[C:12](=[O:14])[S:13][C:9]=2[CH:8]=1)=O.Cl.[CH3:39][O:40][NH2:41].Cl>N1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([C:5](=[N:41][O:40][CH3:39])[C:7]2[CH:34]=[CH:33][C:10]3[N:11]([CH2:15][CH2:16][O:17][C:18]4[CH:19]=[CH:20][C:21]([O:22][C:23]([CH3:29])([CH3:30])[C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:31][CH:32]=4)[C:12](=[O:14])[S:13][C:9]=3[CH:8]=2)[CH:35]=[CH:36][CH:37]=1