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Sodium Hydroxide → HCID 21101214、化合物

HRID 1352851
ノート
印刷プレビュー

反応式

HRID 1352851 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[C:11](OCC)=[O:12])=[CH:5][C:4]=1[O:16][CH2:17][O:18][CH3:19].[OH-].[Na+]>C1(C)C=CC=CC=1.CCCCCC>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[CH2:11][OH:12])=[CH:5][C:4]=1[O:16][CH2:17][O:18][CH3:19]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 89258928HCID 89258928、化合物

生成物 1

HCID 21101214HCID 21101214、化合物収率 95.7%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8058Hexane溶媒

反応条件

温度
-78 °C

実験手順

A solution of the compound (4.54 g, 17.0 mmol) of Example 9-2 in toluene (60 ml) was stirred at −78° C., and thereto was dropped diisobutylalminumhydride (1.0M in hexane: 35.8 ml, 35.8 mmol). The mixture was stirred for 1.5 hours at −78° C., followed by addition of an aqueous 2N sodium hydroxide solution. The precipitate was filtered off and the filtrate was extracted with ethyl acetate. The organic layer was washed with water and an aqueous sodium chloride solution in the order, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the subject compound (3.65 g, 95.7%).

後処理

  1. filtrationThe precipitate was filtered off
  2. extractionthe filtrate was extracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialan aqueous sodium chloride solution in the order, and dried over anhydrous magnesium sulfate
  5. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-02cfd4d2298b4381a26ca2fb55c4e089
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07220773B2

反応ノート

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