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Lithium hydride → HCID 59496799、化合物

HRID 416984
ノート
印刷プレビュー

反応式

HRID 416984 の反応式
[CH2:1]([O:3][C:4](=[O:29])[CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]Br)[C:10]=1[CH2:22][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH3:2].[Br:30][C:31]1[CH:32]=[C:33]([OH:38])[CH:34]=[C:35]([OH:37])[CH:36]=1.[H-].[Li+]>CS(C)=O.O>[CH2:1]([O:3][C:4](=[O:29])[CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][O:37][C:35]2[CH:34]=[C:33]([OH:38])[CH:32]=[C:31]([Br:30])[CH:36]=2)[C:10]=1[CH2:22][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 62714Lithium hydrideHCID 5573835-BromoresorcinolHCID 575864914-[3-(6-Bromo-hexyl)-2-(ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester

生成物 1

HCID 59496799HCID 59496799、化合物収率 74%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962
Water
溶媒

実験手順

To a solution of 4-[3-(6-bromo-hexyl)-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (4.48 g, 9.5 mmol) and 5-bromo-benzene-1,3-diol (1.79 g, 9.47 mmol) in dimethylsulfoxide (30 mL) was added lithium hydride (160 mg, 20 mmol) at room temperature. The resulting suspension was stirred for 48 h and then the reaction mixture was diluted with water (100 mL). The organic compound was extracted into ethyl acetate (3×50 mL) and the combined organic extracts were washed with water (100 mL) and brine solution (100 mL). The organic layers were dried over anhydrous magnesium sulfate and filtration of the drying agent and concentration of the solvent under vacuum gave the crude product which was purified by using an ISCO 120 g column, eluting with 0-30% ethyl acetate in hexanes to afford 4-[3-[6-(3-bromo-5-hydroxy-phenoxy)-hexyl]-2-(2-ethoxycarbonyl-ethyl)-phenoxy]-butyric acid ethyl ester (2.73 g, 74%) as a white solid: ES(+)-HRMS m/e calcd for C29H39BrO7 (M+Na)+ 601.1771, found 601.1773.

後処理

  1. extractionThe organic compound was extracted into ethyl acetate (3×50 mL)
  2. washthe combined organic extracts were washed with water (100 mL) and brine solution (100 mL)
  3. dry with materialThe organic layers were dried over anhydrous magnesium sulfate and filtration of the drying agent and concentration of the solvent under vacuum
  4. customgave the crude product which
  5. customwas purified
  6. washeluting with 0-30% ethyl acetate in hexanes

出典と根拠

ORDレコード
ord-c9717640fc3046d8982624cd75bd0651
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08088936B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート