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

HRID 12176

반응식

HRID 12176 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 225963353-(2-Aminophenoxy)benzonitrile수율 99%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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 C13H11N2O (M+H)+: 211.

후처리

  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

출처 및 근거

ORD 기록
ord-a8a6e596c40a42de81190832f7c60776
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727981B2

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