Phosgene → HCID 88493185、化合物
反応式
[CH2:1]([C:3]1[N:4]=[CH:5][S:6][C:7]=1[C:8]([OH:10])=O)[CH3:2].C(Cl)([Cl:13])=O>C1(C)C=CC=CC=1>[CH2:1]([C:3]1[N:4]=[CH:5][S:6][C:7]=1[C:8]([Cl:13])=[O:10])[CH3:2]参加物
4
実験手順
In a similar apparatus to Example 1,7.9 g (0.05 mole) of 4-ethylthiazole-5carboxylic acid were suspended in 100 ml of toluene. Under heating and reflux, phosgene was blown at a rate of 220 ml/hr for 15 hours (0.15 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 8.5 g of 4-ethylthiazole-5carboxylic acid chloride. Its purity and yield were 95.0% and 92.0%, respectively. NMR (δCDCl 3/TMS, ppm): 1.28(3H,t,J=7Hz), 3.10(2H,q,J=7Hz).
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-a3138741e6ce428bac371dfc9150397e
- 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…