反应详情

温度

0 °C

Oxalyl chloride (2.8 mL, 32.1 mmol) was added over a period of 10 min to a solution of (1S,4S)-4,7,7-trimethyl-3-oxo-bicyclo[2.2.1]heptane-2-carboxylic acid (Intermediate 24; 2.1 g, 10.7 mmol) and N,N-dimethylformamide (3 drops) in dichloromethane (15 mL) at 0° C. The reaction mixture was stirred at 0° C. for 5 min and then at room temperature for 2 h. The solvent was evaporated, and the residue was co-evaporated three times with dichloromethane and then dried under high vacuum for 20 min to give (1S,4S)-4,7,7-trimethyl-3-oxo-bicyclo[2.2.1]heptane-2-carbonyl chloride (2.2 g, 96%) as an orange oil. This was used directly in subsequent steps without further purification.

1. waitat room temperature for 2 h
2. customThe solvent was evaporated
3. customdried under high vacuum for 20 min