反应详情

The above amino amide (50 mg, 0.15 mmol) was added to a solution of benzoyl chloride (32 mg, 0.23 mmol) in THF (1 mL). Triethylamine (0.03 mL, 0.23 mmol) was added and the mixture stirred for 1 h. TLC showed conversion to the benzamide. The solvent was evaporated and the residue dissolved in MeOH (1 mL). Sodium methoxide in MeOH (25%, 0.2 mL) was added and the solution heated to reflux for 45 min. The cooled mixture was partitioned between 1M NH4Cl and CH2Cl2. The residue from the organic layer was stirred and refluxed with MeOH (2 mL) for 1 h, cooled, filtered and washed with MeOH to yield the title compound, 7 (52 mg, 79%) Mp>300° C. MS (ES+) 436,438 (MH+).

1. customThe solvent was evaporated
2. dissolutionthe residue dissolved in MeOH (1 mL)
3. additionSodium methoxide in MeOH (25%, 0.2 mL) was added
4. temperaturethe solution heated
5. temperatureto reflux for 45 min
6. customThe cooled mixture was partitioned between 1M NH4Cl and CH2Cl2
7. stirringThe residue from the organic layer was stirred
8. temperaturerefluxed with MeOH (2 mL) for 1 h
9. temperaturecooled
10. filtrationfiltered
11. washwashed with MeOH