Phosgene → HCID 14716204、化合物
反応式
[CH3:1][O:2][C:3]1[S:4][C:5]([C:9]([OH:11])=O)=[C:6]([CH3:8])[N:7]=1.C(Cl)([Cl:14])=O>ClC1C=CC=CC=1>[CH3:1][O:2][C:3]1[S:4][C:5]([C:9]([Cl:14])=[O:11])=[C:6]([CH3:8])[N:7]=1参加物
4
実験手順
In a similar apparatus to Example 1, 10.4 g (0.06 mole) of 2-methoxy-4-methylthiazole-5-carboxylic acid were suspended in 150 ml of chlorobenzene. Under heating and reflux, phosgene was blown at a rate of 400 ml/hr for 15 hours (0.27 mole). After completion of the blowing, stirring was continued for additional 2 hours. After completion of the reaction, the reaction mixture was filtered and the filtrate was concentrated to obtain 10.9 g of 2-methoxy-4-methylthiazole-5-carboxylic acid chloride. Its purity and yield were 95.0% and 90.0%, respectively. NMR (δCDCl 3/TMS, ppm): 2.70(3H,s), 3.85(3H,s).
後処理
- temperatureUnder heating
- temperaturereflux
- customAfter completion of the reaction
- filtrationthe reaction mixture was filtered
- concentrationthe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-3e82054883a14b9085202ccca8896948
- 出典データセット
- uspto-grants-1992_08
- 特許番号
- US05136042
反応ノート
読み込み中…