반응 #527147
ord-ca8ed3eaa5d74164ae370892321bb77f
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1세척The reaction mixture is washed with water
- 2건조the organic layer dried with Na2SO4
- 3workup.ADDITIONHexane is added at the boil
실험 절차
A solution of 0.83 g of 10,11-dihydro-10-(4-amino-3-methylbenzoyl)-5H-pyrrolo[2,1-c][1,4]benzodiazepine, 0.5 g of N,N-diisopropylethylamine and 0.6 g of 2-methylbenzoyl chloride in 50 ml of methylene chloride is stirred at room temperature for 18 hours. The reaction mixture is washed with water, the organic layer dried with Na2SO4 and passed through a pad of hydrous magnesium silicate. Hexane is added at the boil to give 0.75 g of a solid which is crystallized from methylene chloride-hexane to give 0.61 g of the desired product, m.p. 125°-130° C.