Dimethylformamide → 3-Chloro-5-methylthiophene-2-carbonyl chloride
反応式
[C:1]([C:4]1[S:5][C:6]([CH3:10])=[CH:7][C:8]=1[Cl:9])(O)=[O:2].C(Cl)(=O)C([Cl:14])=O.CN(C=O)C>C(Cl)Cl>[Cl:14][C:1]([C:4]1[S:5][C:6]([CH3:10])=[CH:7][C:8]=1[Cl:9])=[O:2]参加物
5
実験手順
To a suspension of 2-carboxy-3-chloro-5-methylthiophene (1.2 g, 6.6 mmol) in methylene chloride (16 mL) at 0° C. were added oxalyl chloride (0.6 mL, 7.3 mmol) and a drop of DMF. The mixture was stirred at ambient temperature for 5 hours, then concentrated of all volatiles and dried in vacuo to afford 1.3 g (quantitative yield) of 2-chlorocarbonyl-3-chloro-5-methylthiophene as a pale yellow solid; NMR (DMSO-d6/TFA) 7.4 (s, 1), 2.5 (s, 3) ppm.
後処理
- concentrationconcentrated of all volatiles
- customdried in vacuo
出典と根拠
- ORDレコード
- ord-3db0c2fe1c4e4c54bc99775bd1bc0d11
- 出典データセット
- uspto-grants-2002_04
- 特許番号
- US06380221B1
反応ノート
読み込み中…