Ammonium formate → HCID 22380663, 화합물

HRID 895647노트

반응식

HRID 895647 반응식
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

참가 물질

5

반응물 2

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

생성물 1

HCID 22380663HCID 22380663, 화합물수율 73.3%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

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%.

후처리

  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)

출처 및 근거

ORD 기록
ord-4576680ac5d542658cb4b108f8e82f1f
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06916822B2

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