HRID348681

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID6598

Dimethylcarbamoyl chloride

C3H6ClNO

结构：CCCN(CCC)Cc1ccc(NC(=O)c2ccc(CN(Cc3ncc[nH]3)Cc3nccn3C)cc2)cc1

HCID11950262

未命名化合物

PRODUCTS

生成物

结构：CCCN(CCC)Cc1ccc(NC(=O)c2ccc(CN(Cc3nccn3C)Cc3nccn3C(=O)N(C)C)cc2)cc1

HCID58801891

未命名化合物

收率 42%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID1049

Pyridine

C5H5N

PROCEDURE

实验过程

The compound (95.0 mg) obtained in Example 49-1 was dissolved in pyridine (5.0 ml) and added with N,N-dimethylcarbamoyl chloride (20.0 mg). After the solution had been stirred at room temperature for 15 hours, pyridine was distilled off and the residue was then added with a saturated aqueous sodium bicarbonate solution and extracted with chloroform. The extract was concentrated and purified through column chromatography (chloroform/methanol), thereby obtaining the subject compound (45.4 mg) as a white solid.

WORKUP

后处理

distillationpyridine was distilled off
additionthe residue was then added with a saturated aqueous sodium bicarbonate solution
extractionextracted with chloroform
concentrationThe extract was concentrated
custompurified through column chromatography (chloroform/methanol)

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-d8aac73f92bb4a3892b73980bb352b1e
来源数据集: uspto-grants-2007_02
DOI: 10.6084/m9.figshare.5104873.v1
专利: US07176227B2
来源说明: uspto-grants-2007_02

反应 SMILES

[CH2:1]([N:4]([CH2:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16](=[O:38])[C:17]2[CH:22]=[CH:21][C:20]([CH2:23][N:24]([CH2:32][C:33]3[NH:34][CH:35]=[CH:36][N:37]=3)[CH2:25][C:26]3[N:27]([CH3:31])[CH:28]=[CH:29][N:30]=3)=[CH:19][CH:18]=2)=[CH:11][CH:10]=1)[CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3].[CH3:39][N:40]([CH3:44])[C:41](Cl)=[O:42]>N1C=CC=CC=1>[CH3:39][N:40]([CH3:44])[C:41]([N:37]1[CH:36]=[CH:35][N:34]=[C:33]1[CH2:32][N:24]([CH2:23][C:20]1[CH:19]=[CH:18][C:17]([C:16](=[O:38])[NH:15][C:12]2[CH:11]=[CH:10][C:9]([CH2:8][N:4]([CH2:5][CH2:6][CH3:7])[CH2:1][CH2:2][CH3:3])=[CH:14][CH:13]=2)=[CH:22][CH:21]=1)[CH2:25][C:26]1[N:27]([CH3:31])[CH:28]=[CH:29][N:30]=1)=[O:42]