Water → 4-Chloro-5-(trifluoromethyl)benzene-1,2-diamine

HRID 53783

反応式

HRID 53783 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([C:12]([F:15])([F:14])[F:13])[C:5]([Cl:11])=[CH:6][C:7]=1[N+:8]([O-])=O.Cl[Sn]Cl.O>C(O)C>[NH2:1][C:2]1[CH:3]=[C:4]([C:12]([F:15])([F:13])[F:14])[C:5]([Cl:11])=[CH:6][C:7]=1[NH2:8]

参加物

5

反応物 3

HCID 962WaterHCID 24479Stannous ChlorideHCID 27376454-Chloro-2-nitro-5-(trifluoromethyl)aniline

生成物 1

HCID 27734974-Chloro-5-(trifluoromethyl)benzene-1,2-diamine収率 71%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
90 °C

実験手順

To a stirred mixture of 3-amino-6-chloro-4-nitrobenzotrifluoride (300 mg, 1.25 mmol) in ethanol (5 mL) was added SnCl2.2 H2O (1.40 g, 6.20 mmol) in one portion. The mixture was refluxed at 80° C. (oil bath, 90° C.) for 1 h and the solution was cooled to room temperature and ice water (20 g) was added. It was adjusted to pH=7 and extracted with ethyl acetate. The extract was dried over Mg2SO4 and evaporated to give 185 mg (71%) of 3,4-diamino-6-chlorobenzotrifluoride as a brown solid. 1H NMR (CDCl3): δ 3.404 (s, 2H); 3.717 (s, 2H); 6.754 (s, 1H); 6.974 (s, 1H).

後処理

  1. temperaturethe solution was cooled to room temperature
  2. extractionextracted with ethyl acetate
  3. dry with materialThe extract was dried over Mg2SO4
  4. customevaporated

出典と根拠

ORDレコード
ord-f868b29587a64c158f258690e36c6f9f
出典データセット
uspto-grants-1997_04
特許番号
US05620979

関連ノート

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