Hydrochloric Acid → HCID 86611028、化合物

HRID 2245917ノート

反応式

HRID 2245917 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@:8]2([O:17][C@H:16]([CH2:18][OH:19])[C@@H:14]([OH:15])[C@H:12]([OH:13])[C@H:10]2[OH:11])[OH:9])=[CH:4][C:3]=1[CH2:20][C:21]1[CH:26]=[CH:25][C:24]([O:27][C:28]2([C:33]([O:35]C)=[O:34])[CH2:32][CH2:31][CH2:30][CH2:29]2)=[CH:23][CH:22]=1.Cl>[OH-].[K+].CO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@:8]2([O:17][C@H:16]([CH2:18][OH:19])[C@@H:14]([OH:15])[C@H:12]([OH:13])[C@H:10]2[OH:11])[OH:9])=[CH:4][C:3]=1[CH2:20][C:21]1[CH:22]=[CH:23][C:24]([O:27][C:28]2([C:33]([OH:35])=[O:34])[CH2:32][CH2:31][CH2:30][CH2:29]2)=[CH:25][CH:26]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 86611027HCID 86611027、化合物

生成物 1

HCID 86611028HCID 86611028、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 14797Potassium Hydroxide溶媒

実験手順

A solution of 1-chloro-4-(β-D-glucopyranos-1-yl)-2-[4-(1-methoxycarbonyl-cyclopent-1-yloxy)-benzyl]-benzene (0.20 g) in aqueous potassium hydroxide solution (4 mol/l, 5 mL) and methanol (5 mL) is stirred at ambient temperature for 4 h. After neutralizing with aqueous hydrochloric acid (1 mol/l), the mixture is concentrated under reduced pressure, diluted with aqueous NaHCO3 solution and extracted with ethyl acetate. The combined organic phases are dried (Na2SO4), the solvent is removed and the residue is purified by chromatography on silica gel (dichloromethane/methanol 1:0→4:1).

後処理

  1. concentrationthe mixture is concentrated under reduced pressure
  2. additiondiluted with aqueous NaHCO3 solution
  3. extractionextracted with ethyl acetate
  4. dry with materialThe combined organic phases are dried (Na2SO4)
  5. customthe solvent is removed
  6. customthe residue is purified by chromatography on silica gel (dichloromethane/methanol 1:0→4:1)

出典と根拠

ORDレコード
ord-44100a696ad041a68304f0e21641b32b
出典データセット
uspto-grants-2010_03
特許番号
US07683160B2

反応ノート

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