Ammonium formate → HCID 22380663、化合物

HRID 895647ノート

反応式

HRID 895647 の反応式
C(O[CH:5]([C:14]1[CH:19]=[CH:18][C:17]([C:20]2[O:21][CH2:22][C:23]([CH3:26])([CH3:25])[N:24]=2)=[CH:16][CH:15]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[O:12][CH3:13])(=O)C.C([O-])=O.[NH4+]>CO.[Pd]>[CH3:25][C:23]1([CH3:26])[CH2:22][O:21][C:20]([C:17]2[CH:18]=[CH:19][C:14]([CH2:5][C:6]3[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=3[O:12][CH3:13])=[CH:15][CH:16]=2)=[N:24]1

参加物

5

反応物 2

HCID 2723923Ammonium formateHCID 223807461-[4-(4,4-Dimethyloxazolin-2-yl)phenyl]-1-(2-methoxyphenyl)methyl acetate

生成物 1

HCID 22380663HCID 22380663、化合物収率 73.3%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

In an amount of 23.5 mg of the 1-[4-(4,4-dimethyloxazolin-2-yl)phenyl]-1-(2-methoxyphenyl)methyl acetate obtained above was dissolved in methanol (0.47 ml), added with 10% palladium/carbon (24 mg) and ammonium formate (42 mg) under argon atmosphere and stirred at 60° C. for 2 hours. After insoluble matters were removed by filtration, the solvent was evaporated under reduced pressure. The residue was purified by preparative thin layer silica gel column chromatography (developing solvent: hexane:ethyl acetate=1:1) to obtain 14.4 mg of the title compound. Yield: 73%.

後処理

  1. customAfter insoluble matters were removed by filtration
  2. customthe solvent was evaporated under reduced pressure
  3. customThe residue was purified by preparative thin layer silica gel column chromatography (developing solvent: hexane:ethyl acetate=1:1)

出典と根拠

ORDレコード
ord-4576680ac5d542658cb4b108f8e82f1f
出典データセット
uspto-grants-2005_07
特許番号
US06916822B2

反応ノート

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