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

HRID 49529

反応式

HRID 49529 の反応式
[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]

参加物

5

反応物 2

HCID 110573402-Methoxy-5-nitro-N-[[4-(trifluoromethyl)phenyl]methyl]-benzamideHCID 178418361HCID 178418361、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-25d59156999542fc86b97840bb693afb
出典データセット
uspto-grants-2004_03
特許番号
US06706763B1

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