HRID1196540

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID8471

Triethylamine

C6H15N

HCID15592151

未命名化合物

HCID19898933

未命名化合物

PRODUCTS

生成物

结构：Cc1nn(CCN(C)CC(=O)c2ccc(NS(C)(=O)=O)cc2)c(=O)c2ccccc12.Cc1nn(CCN(C)CC(=O)c2ccc(NS(C)(=O)=O)cc2)c(=O)c2ccccc12.O

HCID131716101

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID702

Ethanol

C2H6O

PROCEDURE

实验过程

2-(4-Methyl-2H-phthalazin-1-on-2-yl)-N-methylethylamine hydrobromide (2 g), 4-methanesulphonamidophenacyl bromide (1.8 g) and triethylamine (1.5 g) in ethanol (50 ml) were stirred at room temperature for 2 hours. The solvent was removed, the residue taken up in methylene chloride (100 ml), washed (aqueous sodium bicarbonate), dried (MgSO4) and evaporated. Chromatography on silica [Merck `Kieselgel 60` (Trade Mark)] eluting with methylene chloride containing methanol (0% up to 5%) gave, after collection and evaporation of appropriate fractions, an oil which was triturated with ethanol to give the title compound, yield 1.63 g, m.p. 176°-179°.

WORKUP

后处理

customThe solvent was removed
washwashed (aqueous sodium bicarbonate)
dry with materialdried (MgSO4)
customevaporated
washChromatography on silica [Merck `Kieselgel 60` (Trade Mark)] eluting with methylene chloride
additioncontaining methanol (0% up to 5%)
customgave
customafter collection and evaporation of appropriate fractions
customan oil which was triturated with ethanol

来源与证据

来源类型: Open Reaction Database
ORD 记录: ord-a389401727204960a2fb5c1357c33315
来源数据集: uspto-grants-1992_05
DOI: 10.6084/m9.figshare.5104873.v1
专利: US05114952
来源说明: uspto-grants-1992_05

反应 SMILES

Br.[CH3:2][C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6](=[O:13])[N:5]([CH2:14][CH2:15][NH:16][CH3:17])[N:4]=1.[CH3:18][S:19]([NH:22][C:23]1[CH:32]=[CH:31][C:26]([C:27](=[O:30])[CH2:28]Br)=[CH:25][CH:24]=1)(=[O:21])=[O:20].C(N(CC)CC)C>C(O)C>[OH2:13].[CH3:18][S:19]([NH:22][C:23]1[CH:32]=[CH:31][C:26]([C:27](=[O:30])[CH2:28][N:16]([CH2:15][CH2:14][N:5]2[N:4]=[C:3]([CH3:2])[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[C:6]2=[O:13])[CH3:17])=[CH:25][CH:24]=1)(=[O:21])=[O:20].[CH3:18][S:19]([NH:22][C:23]1[CH:32]=[CH:31][C:26]([C:27](=[O:30])[CH2:28][N:16]([CH2:15][CH2:14][N:5]2[N:4]=[C:3]([CH3:2])[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[C:6]2=[O:13])[CH3:17])=[CH:25][CH:24]=1)(=[O:21])=[O:20]