Dichloromethane → HCID 18182320、化合物

HRID 1359413ノート

反応式

HRID 1359413 の反応式
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

参加物

6

反応物 3

HCID 6344DichloromethaneHCID 5003444Sodium cyanoborohydrideHCID 18182224HCID 18182224、化合物

生成物 1

HCID 18182320HCID 18182320、化合物収率 74.9%

試薬・触媒・溶媒 2

HCID 9883512zinc(II)iodide触媒HCID 887Methanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-d1090ac100cc49bfb0d0601bb096aff4
出典データセット
uspto-grants-2003_07
特許番号
US06599917B1

反応ノート

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