反応式
CS([Cl:5])(=O)=O.[Cl:6][C:7]1[CH:30]=[CH:29][C:10]([CH2:11][NH:12][C:13]([C:15]2[C:16](=[O:28])[C:17]3[S:24][C:23]([CH2:25]O)=[C:22]([CH3:27])[C:18]=3[N:19]([CH3:21])[CH:20]=2)=[O:14])=[CH:9][CH:8]=1.N1C(C)=CC(C)=CC=1C>CN(C1C=CN=CC=1)C.CN(C=O)C.O>[Cl:6][C:7]1[CH:8]=[CH:9][C:10]([CH2:11][NH:12][C:13]([C:15]2[C:16](=[O:28])[C:17]3[S:24][C:23]([CH2:25][Cl:5])=[C:22]([CH3:27])[C:18]=3[N:19]([CH3:21])[CH:20]=2)=[O:14])=[CH:29][CH:30]=1参加物
7
反応物 3
生成物 1
試薬・触媒・溶媒 3
実験手順
Methanesulfonyl chloride (0.23 mL, 3.0 mmol) was added to a mixture of N-(4-chlorobenzyl)-2-(hydroxymethyl)-3,4-dimethyl-7-oxo-4,7-dihydrothieno[3,2-b]pyridine-6-carboxamide (446 mg, 1.19 mmol), collidine (0.39 mL, 3.0 mmol) and DMAP (22 mg, 0.18 mmol) in DMF (21 mL). The reaction was stirred at room temperature for 1 hour 15 minutes, going to an orange/amber solution. The reaction was cooled in an ice bath before diluting with water to a total volume of 100 mL. The mixture was stirred vigorously for 5 minutes before the solid precipitate was collected by filtration, washed with water and dried in vacuo, leaving the title compound as a white solid (460 mg).
後処理
- temperatureThe reaction was cooled in an ice bath
- stirringThe mixture was stirred vigorously for 5 minutes before the solid precipitate
- filtrationwas collected by filtration
- washwashed with water
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-59650167e48a4e9ca71d5bf04906a654
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06852731B2
関連ノート
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