Water → HCID 131728196, 화합물

HRID 19833노트

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HRID 19833 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 131728196HCID 131728196, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 57417360Sodium chloride; water용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-048665e75f7845788f889966428dc5d0
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745414B2

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