Dichloromethane → HCID 18182320, 화합물

HRID 1359413노트

반응식

HRID 1359413 반응식
O[CH:2]([C:9]1[C:10]2[CH2:17][CH2:16][CH:15]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:14][C:11]=2[S:12][CH:13]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C([BH3-])#N.[Na+].ClCCl>[I-].[Zn+2].[I-].CO>[CH2:2]([C:9]1[C:10]2[CH2:17][CH2:16][CH:15]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH2:14][C:11]=2[S:12][CH:13]=1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 5003444Sodium cyanoborohydrideHCID 18182224HCID 18182224, 화합물

생성물 1

HCID 18182320HCID 18182320, 화합물수율 74.9%

시약·촉매·용매 2

HCID 9883512zinc(II)iodide촉매HCID 887Methanol용매

실험 절차

A mixture of 8.3 g of 3-(α-hydroxybenzyl)-6-ethoxycarbonyl-4,5,6,7-tetrahydrobenzo[b]thiophene, 12.5 g of zinc iodide, 2.0 g of sodium cyanoborohydride and 150 ml of dichloromethane was stirred at room temperature for 3 hours. After adding methanol to the reaction solution, insoluble matters were filtered off. The solvent was removed, and the residue was subjected to silica gel column chromatography and eluted with hexane and then with hexane/ethyl acetate (10:1), to give 5.9 g of the target compound.

후처리

  1. filtrationwere filtered off
  2. customThe solvent was removed
  3. washeluted with hexane

출처 및 근거

ORD 기록
ord-d1090ac100cc49bfb0d0601bb096aff4
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06599917B1

반응 노트

불러오는 중…