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Ammonium formate → (4-Amino-2-phenylbenzoyl)methionine 2-trimethylsilylethyl ester

HRID 383128
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HRID 383128 반응식
[CH3:1][Si:2]([CH3:32])([CH3:31])[CH2:3][CH2:4][O:5][C:6](=[O:30])[C@H:7]([CH2:26][CH2:27][S:28][CH3:29])[NH:8][C:9](=[O:25])[C:10]1[CH:15]=[CH:14][C:13]([N+:16]([O-])=O)=[CH:12][C:11]=1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C([O-])=O.[NH4+]>CO.[Pd]>[CH3:32][Si:2]([CH3:1])([CH3:31])[CH2:3][CH2:4][O:5][C:6](=[O:30])[C@H:7]([CH2:26][CH2:27][S:28][CH3:29])[NH:8][C:9](=[O:25])[C:10]1[CH:15]=[CH:14][C:13]([NH2:16])=[CH:12][C:11]=1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 2723923Ammonium formateHCID 69844218(4-Nitro-2-phenylbenzoyl)methionine 2-trimethylsilylethyl ester

생성물 1

HCID 67550574(4-Amino-2-phenylbenzoyl)methionine 2-trimethylsilylethyl ester

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A mixture of the product of Example 283A (8.85 g, 25.8 mmol), ammonium formate (4.88 g, 77.4 mmol) and palladium (10%) on carbon (1 g) in methanol was refluxed for 5 hours. The mixture was then filtered through Celite and rinsed with ethyl acetate. The filtrate was diluted with ethyl acetate, washed with water and brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to give the title compound which was used without further purification.

후처리

  1. temperaturewas refluxed for 5 hours
  2. filtrationThe mixture was then filtered through Celite
  3. washrinsed with ethyl acetate
  4. additionThe filtrate was diluted with ethyl acetate
  5. washwashed with water and brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-82ba6c1decc94e86a7cdd5d6c8b2bfd1
출처 데이터셋
uspto-grants-2001_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06310095B1

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