Imidazole → 6-methyl-1H-inden-1,2(3H)-dione 2-{O-[tert-butyl(dimethyl)silyl]oxime}

HRID 1893512ノート

反応式

HRID 1893512 の反応式
CN(C)C=O.[CH3:6][C:7]1[CH:15]=[C:14]2[C:10]([CH2:11][C:12](=[N:17][OH:18])[C:13]2=[O:16])=[CH:9][CH:8]=1.N1C=CN=C1.[Si:24](Cl)([C:27]([CH3:30])([CH3:29])[CH3:28])([CH3:26])[CH3:25]>O>[Si:24]([O:18][N:17]=[C:12]1[CH2:11][C:10]2[C:14](=[CH:15][C:7]([CH3:6])=[CH:8][CH:9]=2)[C:13]1=[O:16])([C:27]([CH3:30])([CH3:29])[CH3:28])([CH3:26])[CH3:25]

参加物

6

反応物 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 28928tert-Butyldimethylsilyl chlorideHCID 587173366-Methyl-2-hydroxyimino-1-indanone

生成物 1

HCID 866507766-methyl-1H-inden-1,2(3H)-dione 2-{O-[tert-butyl(dimethyl)silyl]oxime}収率 83.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
95 °C

実験手順

To N,N-dimethylformamide (50 ml) were added at room temperature the compound (4.36 g, 24.9 mmol) obtained in step A, imidazole (5.10 g, 74.7 mmol) and tert-butyldimethylsilyl chloride (5.60 g, 37.4 mmol), and the mixture was stirred at 95° C. for 2 hr. After cooling to room temperature, water was added to the reaction solution with stirring and the precipitated solid was filtered, washed with water, and dried under reduced pressure to give the title compound (6.00 g, yield 83%) as a pale-bistered solid.

後処理

  1. temperatureAfter cooling to room temperature
  2. stirringwith stirring
  3. filtrationthe precipitated solid was filtered
  4. washwashed with water
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-993fdb9e18814b24aa804676ec771d1c
出典データセット
uspto-grants-2013_08
特許番号
US08513235B2

反応ノート

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