Tetrahydrofuran → HCID 66810488、化合物

HRID 1097530ノート

反応式

HRID 1097530 の反応式
[C:1]([C:3]1[CH:30]=[C:29]([N+:31]([O-])=O)[CH:28]=[CH:27][C:4]=1[O:5][C:6]1[CH:7]=[CH:8][C:9]([F:26])=[C:10]([NH:12][C:13](=[O:25])[CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=2)[CH:11]=1)#[N:2].O1CCCC1>C(O)C.[C].[Pd]>[NH2:31][C:29]1[CH:28]=[CH:27][C:4]([O:5][C:6]2[CH:7]=[CH:8][C:9]([F:26])=[C:10]([NH:12][C:13](=[O:25])[CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:22])([F:23])[F:24])[CH:16]=3)[CH:11]=2)=[C:3]([C:1]#[N:2])[CH:30]=1

参加物

5

反応物 2

HCID 8028TetrahydrofuranHCID 66810481HCID 66810481、化合物

生成物 1

HCID 66810488HCID 66810488、化合物収率 92.1%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 702Ethanol溶媒

実験手順

To a solution of N-[5-(2-cyano-4-nitrophenoxy)-2-fluorophenyl]-2-[3-(trifluoromethyl)phenyl]acetamide (1.36 g, 2.96 mmol) in ethanol (25 mL)/tetrahydrofuran (10 mL) was added 10% palladium-carbon (160 mg), and the mixture was stirred at room temperature for 5 hr under a hydrogen atmosphere (1 atm). Insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by basic silica gel column chromatography (ethyl acetate/n-hexane=30/70→100/0), and the fraction containing the object product was concentrated under reduced pressure to give the title compound (1.17 g, 92%) as a beige amorphous form.

後処理

  1. filtrationInsoluble material was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe obtained residue was purified by basic silica gel column chromatography (ethyl acetate/n-hexane=30/70→100/0)
  4. additionthe fraction containing the object product
  5. concentrationwas concentrated under reduced pressure

出典と根拠

ORDレコード
ord-3efbea28dba445f2bb657ff4452bc841
出典データセット
uspto-grants-2012_03
特許番号
US08143258B2

反応ノート

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