Water → 4-Trifluoromethyl-1,2-phenylenediamine

HRID 54407

反応式

HRID 54407 の反応式
[N+:1]([C:4]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:8]=[CH:7][C:5]=1[NH2:6])([O-])=O.Cl[Sn]Cl.O.C([O-])(O)=O.[Na+]>C(O)C>[F:12][C:11]([F:13])([F:14])[C:9]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([NH2:1])[CH:10]=1

参加物

6

反応物 4

HCID 962WaterHCID 24479Stannous ChlorideHCID 67865Benzenamine, 2-nitro-4-(trifluoromethyl)-HCID 516892Sodium Bicarbonate

生成物 1

HCID 5208224-Trifluoromethyl-1,2-phenylenediamine収率 96.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-nitro-4-trifluoromethylaniline (5.000 g, 24.26 mmol, Aldrich, used as received) and SnCl2.2 H2O (20.00 g, 88.64 mmol, Aldrich, used as received) in absolute ethanol (50 mL) was refluxed for 45 min. It was then poured into ice (85 g) and basified with 10% aq. NaHCO3 (250 mL). The resulting suspension was extracted with ethyl acetate (400 mL). The ethyl acetate extract was dried over Na2SO4 and evaporated to give 4.14 g (87%) of pure 4-trifluoromethyl-1,2-phenylenediamine as a red powder.

後処理

  1. extractionThe resulting suspension was extracted with ethyl acetate (400 mL)
  2. extractionThe ethyl acetate extract
  3. dry with materialwas dried over Na2SO4
  4. customevaporated

出典と根拠

ORDレコード
ord-62109381f5f14189913bf106ba37e015
出典データセット
uspto-grants-1997_04
特許番号
US05622952

関連ノート

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