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Ammonia → 2-Amino-6-(trifluoromethyl)benzamide

HRID 1294559
ノート
印刷プレビュー

反応式

HRID 1294559 の反応式
F[C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([F:13])([F:12])[F:11])[C:3]=1[C:4]#[N:5].[NH3:14].OS(O)(=O)=O.[OH-:20].[Na+]>CO>[NH2:14][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]([F:13])([F:12])[F:11])[C:3]=1[C:4]([NH2:5])=[O:20]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 222AmmoniaHCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 1456132-Fluoro-6-(trifluoromethyl)benzonitrile

生成物 1

HCID 198263532-Amino-6-(trifluoromethyl)benzamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
100 °C

実験手順

100 mg (0.5 mmol) 2-fluoro-6-trifluoromethyl-benzonitrile are combined with 1 ml of a 7 M ammonia solution in methanol and heated in the microwave for 20 min. at 100° C. Then the solvent is eliminated in vacuo, the crude product is combined with 1 ml of conc. H2SO4 and heated for 2.5 h at 80° C. Then the reaction mixture is stirred into ice water, neutralised with 1 M NaOH and extracted twice with 150 ml dichloromethane and three times with 160 ml of ethyl acetate. The organic phase is dried with MgSO4 and the solvent is eliminated in vacuo. The crude product is purified by column chromatography. The carrier material used is silica gel and the eluant is dichloromethane, to which 4% of a mixture of 90% methanol and 10% saturated aqueous ammonia solution have been added.

後処理

  1. temperatureheated for 2.5 h at 80° C
  2. extractionextracted twice with 150 ml dichloromethane and three times with 160 ml of ethyl acetate
  3. dry with materialThe organic phase is dried with MgSO4
  4. customThe crude product is purified by column chromatography
  5. additionto which 4% of a mixture of 90% methanol and 10% saturated aqueous ammonia solution have been added

出典と根拠

ORDレコード
ord-7ebe0fca9c804060bc250786364ed9aa
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07241769B2

反応ノート

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