反应详情

The carboxylic acid from Example 12 (0.5 g, 1.25 mmol) in dichloromethane (10 ml) was treated with oxalyl chloride (0.3 ml, 3.4 mol) and DMF (catalytic). Solution was stirred for 1 h and evaporated to dryness. The residue in dry THF (5 ml) was added to a stirred solution of triethylamine (0.3 ml, 4 mmol) and N,N,N'-trimethylethylenediamine (0.5 ml, 4.5 mmol) in dry THF (10 ml). Following 3 hours at room temperature, the solution was partitioned (H2O/EtOAc). Drying and removal of the organic layers followed by recrystallisation (EtOAc/60°-80° petrol) afforded the title compound (0.5 g, 83%) as a white solid. M.pt. 140°-141° C.

1. customevaporated to dryness
2. waitFollowing 3 hours at room temperature
3. customthe solution was partitioned (H2O/EtOAc)
4. customDrying
5. customremoval of the organic layers
6. customfollowed by recrystallisation (EtOAc/60°-80° petrol)