반응 #308435

반응 방정식

N-trifluoroacetyl-7-hydroxy-8-iodo-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine

allyl bromide

DBU

→

clear oil

수율 69.8%

N-Trifluoroacetyl-7-allyloxy-8-iodo-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine

수율 69.8%

용매

dichloromethane

EtOAc

반응 조건

후처리

1. 1
   세척washed with 5% aqueous HCl (5 mL), brine (5 mL)
2. 2
   건조dried with Na2SO4
3. 3
   농축concentrated

실험 절차

A solution of N-trifluoroacetyl-7-hydroxy-8-iodo-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (30 mg, 0.075 mmol) in dichloromethane (2 mL) was treated with allyl bromide (18 mg, 0.15 mmol), DBU (23 mg, 0.15 mmol) and stirred 2 hours at 20 C. The product mixture was diluted with EtOAc (10 mL), washed with 5% aqueous HCl (5 mL), brine (5 mL), dried with Na2SO4 and concentrated. Flash chromatography (15% EtOAc in hexane, silica) resulted in 23 mg of a clear oil. MS calculated for C16H17F3INO2+H: 440, observed: 440.

출처