Stannous chloride dihydrate → 3-(2-Aminophenoxy)benzonitrile

HRID 12148

反応式

HRID 12148 の反応式
[N+:1]([C:4]1[CH:18]=[CH:17][CH:16]=[CH:15][C:5]=1[O:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][CH:14]=1)[C:10]#[N:11])([O-])=O.O.O.Cl[Sn]Cl>CCO>[NH2:1][C:4]1[CH:18]=[CH:17][CH:16]=[CH:15][C:5]=1[O:6][C:7]1[CH:8]=[C:9]([CH:12]=[CH:13][CH:14]=1)[C:10]#[N:11]

参加物

4

反応物 2

HCID 61436Stannous chloride dihydrateHCID 91948883-(2-Nitrophenoxy)benzonitrile

生成物 1

HCID 225963353-(2-Aminophenoxy)benzonitrile収率 99%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 3-(2-nitrophenoxy)benzonitrile (1.21 g, 5 mmol, 1.0 equiv) in 30 mL of EtOH was treated with SnCl2.2H2O (3.38 g, 3 equiv) at reflux for 4 h. The volatile was evaporated and the residue was redissolved in EtOAc, washed with saturated aqueous NaHCO3 and 1N NaOH. The organic layer was dried over MgSO4, filtered and evaporated to give 3-(2-aminophenoxy)benzonitrile (1.04 g, 99%). MS found for Cl3H11N2O (M+H)+: 211.

後処理

  1. temperatureat reflux for 4 h
  2. customThe volatile was evaporated
  3. dissolutionthe residue was redissolved in EtOAc
  4. washwashed with saturated aqueous NaHCO3 and 1N NaOH
  5. dry with materialThe organic layer was dried over MgSO4
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-23a25129716941e9a600ead660148e17
出典データセット
uspto-grants-2010_06
特許番号
US07727982B2

関連ノート

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