反应详情

N-(2,4-difluorobenzyl)-N-heptyl-2-[4-(2-hydroxyethyl)-2-methoxyphenoxy]acetamide (A)(132 mg, 0.294 mmol) was dissolved in DCM (10 ml). It was cooled in an ice-bath. Triethylamine (0.05 ml, 0.352 mmol) was added and then methanesulfonyl chloride (37 mg, 0.323 mmol) was dropped in. The cooling-bath was removed after 30 minutes. The mixture was stirred at room temperature overnight. LS-MS showed that ca 50% of A was not reacted. The mixture was cooled in an ice-bath and 0.05 ml of triethylamine was added, followed by 0.025 ml of methanesulfonyl chloride. After addition, the cooling-bath was removed and the mixture was stirred for 5 hours more. It was then washed with water (×2) and brine, dried (magnesium sulphate) and evaporated. Oil product 138 mg was left and used for next step without further purification.

1. temperatureIt was cooled in an ice-bath
2. customThe cooling-bath was removed after 30 minutes
3. customwas not reacted
4. temperatureThe mixture was cooled in an ice-bath
5. additionAfter addition
6. customthe cooling-bath was removed
7. stirringthe mixture was stirred for 5 hours more
8. washIt was then washed with water (×2) and brine
9. dry with materialdried (magnesium sulphate)
10. customevaporated
11. waitOil product 138 mg was left
12. customused for next step without further purification