Dimethylformamide → 2-[4-(4-Chlorobenzoyl)benzyl]thio-3,5-dimethylthieno[2,3-d]pyrimidin-4(3H)-one

HRID 1291331ノート

反応式

HRID 1291331 の反応式
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[C:9]([CH3:12])=[CH:10][S:11][C:5]=2[N:4]=[C:3]1[SH:13].[OH-].[Na+].CN(C=O)C.[Cl:21][C:22]1[CH:37]=[CH:36][C:25]([C:26]([C:28]2[CH:35]=[CH:34][C:31]([CH2:32]Br)=[CH:30][CH:29]=2)=[O:27])=[CH:24][CH:23]=1>CO.O>[Cl:21][C:22]1[CH:23]=[CH:24][C:25]([C:26]([C:28]2[CH:35]=[CH:34][C:31]([CH2:32][S:13][C:3]3[N:2]([CH3:1])[C:7](=[O:8])[C:6]4[C:9]([CH3:12])=[CH:10][S:11][C:5]=4[N:4]=3)=[CH:30][CH:29]=2)=[O:27])=[CH:36][CH:37]=1

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 14798Sodium HydroxideHCID 98396514-(4-Chlorobenzoyl)benzyl bromideHCID 178431876HCID 178431876、化合物

生成物 1

HCID 189191282-[4-(4-Chlorobenzoyl)benzyl]thio-3,5-dimethylthieno[2,3-d]pyrimidin-4(3H)-one収率 39.9%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 3,5-dimethyl-2-mercaptothieno[2,3-d]pyrimidin-4(3H)-one (1.06 g) and sodium hydroxide (205 mg) in 50% methanol (16 ml)-DMF (4 ml) was added 4-(4-chlorobenzoyl)benzyl bromide (1.69 g) and the mixture was stirred at room temperature for 1 hour. This reaction mixture was poured in water and the resulting crystals were collected by filtration, rinsed with water, and recrystallized from ethyl acetate to provide the title compound as colorless solid (878 mg).

後処理

  1. filtrationthe resulting crystals were collected by filtration
  2. washrinsed with water
  3. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-1a2e708edc094e94b18bee23c363da57
出典データセット
uspto-grants-1998_05
特許番号
US05753664

反応ノート

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