HRID1710381

反应详情

EQUATION

反应方程式

REACTANTS

反应物

结构：COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1

HCID87949

p-Anisyldithiophosphonic anhydride

C14H14O2P2S4

结构：CN(CC1CCCO1)S(=O)(=O)c1ccc(-c2cnc3[nH]c(CCC4CCCCC(=O)N4)nc3c2)cc1

HCID178482879

未命名化合物

PRODUCTS

生成物

结构：CN(CC1CCCO1)S(=O)(=O)c1ccc(-c2cnc3[nH]c(CCC4CCCCC(=S)N4)nc3c2)cc1

HCID178482880

未命名化合物

收率 95.4%

PROCEDURE

实验过程

The title compound is synthesized as described for 7-[2-(6-{4-cyano-phen-1-yl}-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-azepan-2-thione (compound A2) from 125 mg of N-methyl-4-{2-[2-(7-oxo-azepan-2-yl)-ethyl]-3H-imidazo[4,5-b]pyridin-6-yl}-N-(tetrahydro-furan-2-ylmethyl)-benzenesulfonamide (compound B10) and 104 mg of Lawesson's reagent. Purification by chromatography on flash silica gel (eluent gradient: dichloromethane/0-10 vol. % ethanol) affords 123 mg of the title compound as a waxy solid. ESI-MS: 528.9 (MH+). TLC: Rf=0.43 (dichloromethane/ethanol 10:1 parts by volume).

WORKUP

后处理

customThe title compound is synthesized
customPurification by chromatography on flash silica gel (eluent gradient: dichloromethane/0-10 vol. % ethanol)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-136c488b0abc42d18213055187795a24
来源数据集: uspto-grants-2010_09
DOI: 10.6084/m9.figshare.5104873.v1
专利: US07790710B2
来源说明: uspto-grants-2010_09

反应 SMILES

[CH3:1][N:2]([CH2:31][CH:32]1[CH2:36][CH2:35][CH2:34][O:33]1)[S:3]([C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:13]=[C:14]3[N:20]=[C:19]([CH2:21][CH2:22][CH:23]4[CH2:29][CH2:28][CH2:27][CH2:26][C:25](=O)[NH:24]4)[NH:18][C:15]3=[N:16][CH:17]=2)=[CH:8][CH:7]=1)(=[O:5])=[O:4].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:46])=CC=1>>[CH3:1][N:2]([CH2:31][CH:32]1[CH2:36][CH2:35][CH2:34][O:33]1)[S:3]([C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:13]=[C:14]3[N:20]=[C:19]([CH2:21][CH2:22][CH:23]4[CH2:29][CH2:28][CH2:27][CH2:26][C:25](=[S:46])[NH:24]4)[NH:18][C:15]3=[N:16][CH:17]=2)=[CH:8][CH:7]=1)(=[O:5])=[O:4]