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Imidazole → HCID 59463439、化合物

HRID 2261341
ノート
印刷プレビュー

反応式

HRID 2261341 の反応式
[OH:1][CH2:2][C:3]1[O:7][N:6]=[C:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:4]=1.N1C=CN=C1.[Si:18](Cl)([C:21]([CH3:24])([CH3:23])[CH3:22])([CH3:20])[CH3:19].O>CN(C)C=O>[Si:18]([O:1][CH2:2][C:3]1[O:7][N:6]=[C:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:4]=1)([C:21]([CH3:24])([CH3:23])[CH3:22])([CH3:20])[CH3:19]
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 4

HCID 795ImidazoleHCID 962WaterHCID 28928tert-Butyldimethylsilyl chlorideHCID 8027233Ethyl 5-(hydroxymethyl)isoxazole-3-carboxylate

生成物 1

HCID 59463439HCID 59463439、化合物収率 100.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

14.22 g of ethyl 5-(hydroxymethyl)-isoxazole-3-carboxylate was dissolved in 80 ml of N,N-dimethylformamide, and 6.13 g of imidazole and 13.57 g of t-butyldimethylsilyl chloride were then added. The mixture was stirred at room temperature for 10 hours. After water was added, the reaction mixture was extracted with methyl-t-butyl ether. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure to obtain 23.82 g of ethyl 5-(t-butyldimethylsilanyloxymethyl)-isoxazole-3-carboxylate.

後処理

  1. extractionthe reaction mixture was extracted with methyl-t-butyl ether
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-e2e9052774764584bd2f1389108b2898
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07846956B2

反応ノート

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