Water → HCID 131728196、化合物

HRID 502859ノート

反応式

HRID 502859 の反応式
[CH3:1][O:2][CH2:3][CH2:4]Br.[OH:6][C@:7]1([C:18]2[CH:25]=[CH:24][C:21]([C:22]#[N:23])=[C:20]([CH2:26][C:27]3[CH:32]=[CH:31][C:30]([OH:33])=[CH:29][CH:28]=3)[CH:19]=2)[O:15][C@H:14]([CH2:16][OH:17])[C@@H:12]([OH:13])[C@H:10]([OH:11])[C@H:8]1[OH:9].C(=O)([O-])[O-].[Cs+].[Cs+].O>CN(C)C=O.[Cl-].[Na+].O>[OH:6][C@:7]1([C:18]2[CH:25]=[CH:24][C:21]([C:22]#[N:23])=[C:20]([CH2:26][C:27]3[CH:28]=[CH:29][C:30]([O:33][CH2:4][CH2:3][O:2][CH3:1])=[CH:31][CH:32]=3)[CH:19]=2)[O:15][C@H:14]([CH2:16][OH:17])[C@@H:12]([OH:13])[C@H:10]([OH:11])[C@H:8]1[OH:9]

参加物

7

反応物 4

HCID 962WaterHCID 10796Cesium carbonateHCID 809722-Bromoethyl methyl etherHCID 866102154-(beta-D-glucopyranos-1-yl)-2-(4-hydroxybenzyl)-benzonitrile

生成物 1

HCID 131728196HCID 131728196、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

2-Bromoethyl methyl ether (85 μl) is added to a mixture of 4-(β-D-glucopyranos-1-yl)-2-(4-hydroxybenzyl)-benzonitrile (0.30 g) and cesium carbonate (0.39 g) in 3 mL of dimethylformamide. The mixture is stirred at 80° C. for 16 h, before water and brine are added. The resulting mixture is extracted with ethyl acetate, the combined extracts are dried over sodium sulphate and the solvent is removed under reduced pressure. The residue is purified by chromatography on silica gel (dichloromethane/methanol 1:0->5:1).

後処理

  1. additionare added
  2. extractionThe resulting mixture is extracted with ethyl acetate
  3. dry with materialthe combined extracts are dried over sodium sulphate
  4. customthe solvent is removed under reduced pressure
  5. customThe residue is purified by chromatography on silica gel (dichloromethane/methanol 1:0->5:1)

出典と根拠

ORDレコード
ord-d3f8e0a1bc1749f8904d86c083e8d917
出典データセット
uspto-grants-2010_08
特許番号
US07776830B2

反応ノート

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