反应详情

温度

80 °C

To a mixture of copper (II) chloride (20 g, 0.15 mol) and 90% t-butyl nitrite (24 mL, 0.18 mol) in 500 mL acetonitrile at 60° C. was added in portions ethyl 2-amino-4-thiazolecarboxylate (21 g, 0.12 mol), maintaining the temperature at between 60°-65° C. After the addition, the resulting reaction mixture was heated at 80° C. for 1 h, then cooled to RT and poured into a mixture of water, CH2Cl2 and 25 mL conc HCl. The aq layer was separated and extracted with CH2Cl2. The combined organic layers were washed with water, brine, dried and concentrated to give 21.5 g of ethyl 2-chloro-4-thiazolecarboxylate.

1. temperaturemaintaining the temperature at between 60°-65° C
2. additionAfter the addition
3. customthe resulting reaction mixture
4. temperaturecooled to RT
5. customThe aq layer was separated
6. extractionextracted with CH2Cl2
7. washThe combined organic layers were washed with water, brine
8. customdried
9. concentrationconcentrated