Aluminium lithium hydride → 2-{2-[3,4-Bis(hydroxymethyl)phenoxy]-1-methylethyl}amino-1-(3-chlorophenyl)ethanol

HRID 1901171

反応式

HRID 1901171 の反応式
C[O:2][C:3]([C:5]1[CH:6]=[C:7]([CH:23]=[CH:24][C:25]=1[C:26](OC)=[O:27])[O:8][CH2:9][CH:10]([NH:12][CH2:13][CH:14]([C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([Cl:22])[CH:17]=1)[OH:15])[CH3:11])=O.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[OH:2][CH2:3][C:5]1[CH:6]=[C:7]([CH:23]=[CH:24][C:25]=1[CH2:26][OH:27])[O:8][CH2:9][CH:10]([NH:12][CH2:13][CH:14]([C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([Cl:22])[CH:17]=1)[OH:15])[CH3:11]

参加物

4

実験手順

Following a procedure similar to that described in Example 1, but using 2.53 g of 2-{2-[3,4-bis(methoxycarbonyl)phenoxy]-1-methylethyl}amino-1-(3-chlorophenyl)ethanol (prepared as described in Preparation 20), 0.91 g of lithium aluminum hydride and 100 ml of dry tetrahydrofuran, and then purifying the reaction product by column chromatography through silica gel, using a 5:1 by volume mixture of ethyl acetate and ethanol as the eluent, 1.04 g of the title compound were obtained having an Rf=0.37 (thin layer chromatography over silica gel, using a 5:1 by volume mixture of ethyl acetate and ethanol as the developing solvent).

後処理

  1. custompurifying the reaction product by column chromatography through silica gel
  2. additionby volume mixture of ethyl acetate and ethanol as the eluent

出典と根拠

ORDレコード
ord-d51c4e6e039d4437aa4a58cdc435be34
出典データセット
uspto-grants-1996_11
特許番号
US05576340

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