2-Methoxy-5-nitro-N-[[4-(trifluoromethyl)phenyl]methyl]-benzamide → 5-amino-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide

HRID 49529

반응식

HRID 49529 반응식
[CH3:1][O:2][C:3]1[CH:22]=[CH:21][C:20]([N+:23]([O-])=O)=[CH:19][C:4]=1[C:5]([NH:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]([F:18])([F:17])[F:16])=[CH:11][CH:10]=1)=[O:6].[H][H]>[Pd].C(OCC)(=O)C>[NH2:23][C:20]1[CH:21]=[CH:22][C:3]([O:2][CH3:1])=[C:4]([CH:19]=1)[C:5]([NH:7][CH2:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]([F:17])([F:18])[F:16])=[CH:13][CH:14]=1)=[O:6]

참가 물질

5

반응물 2

HCID 110573402-Methoxy-5-nitro-N-[[4-(trifluoromethyl)phenyl]methyl]-benzamideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 109034245-amino-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide수율 100.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

To 26.6 g of 2-methoxy-5-nitro-N-(4-trifluoromethylbenzyl)benzamide were added 270 ml of ethyl acetate and 2.6 g of 10% palladium on carbon under an atmosphere of argon, then argon was replaced with hydrogen gas, and the mixture was stirred for 8 hours at room temperature under an atmosphere of hydrogen gas. Catalyst was filtered through Celite(Hyflo Super-cel) and, after washed the collected material well with ethyl acetate, the filtrate was concentrated under reduced pressure. The residue obtained was purified by means of column chromatography (silica gel, ethyl acetate) to obtain 24.5 g of 5-amino-2-methoxy-N-(4-trifluoromethylbenzyl)benzamide as colorless crystals.

후처리

  1. filtrationCatalyst was filtered through Celite(Hyflo Super-cel) and,
  2. washafter washed the collected material well with ethyl acetate
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue obtained
  5. customwas purified by means of column chromatography (silica gel, ethyl acetate)

출처 및 근거

ORD 기록
ord-25d59156999542fc86b97840bb693afb
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706763B1

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