Ethanol → [2-(2-Aminoethyl)-4,5-dimethoxyphenyl]acetonitrile

HRID 76325ノート

反応式

HRID 76325 の反応式
[C:1]([CH2:3][C:4]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([O:12][CH3:13])=[CH:6][C:5]=1[CH2:14][CH2:15][NH:16]C(=O)C(F)(F)F)#[N:2].C(O)C.C(=O)([O-])[O-].[K+].[K+]>O>[NH2:2][CH2:1][CH2:3][C:4]1[CH:9]=[C:8]([O:10][CH3:11])[C:7]([O:12][CH3:13])=[CH:6][C:5]=1[CH2:14][C:15]#[N:16]

参加物

5

反応物 3

HCID 702EthanolHCID 11430Potassium CarbonateHCID 86698209N-{2-[2-(cyanomethyl)-4,5-dimethoxyphenyl]ethyl}-2,2,2-trifluoroacetamide

生成物 1

HCID 86698210[2-(2-Aminoethyl)-4,5-dimethoxyphenyl]acetonitrile収率 70.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

Heat, at 50° C., a mixture of N-{2-[2-(cyanomethyl)-4,5-dimethoxyphenyl]ethyl}-2,2,2-trifluoroacetamide (20.5 g, 64.8 mmoles), ethanol (160 mL), potassium carbonate (13.2 g, 97.2 mmoles) and water (40 mL). After being in contact for 1 hour 30 minutes, extract the mixture by adding 200 mL of dichloromethane and 100 mL of saturated aqueous NaCl solution. Extract the aqueous phase with 100 mL of dichloromethane. Combine the organic phases, wash them with saturated aqueous NaCl solution (100 mL), dry them over MgSO4 and carry out drying in vacuo to obtain 10 g of a yellow oil corresponding to the title compound.

後処理

  1. extractionextract the mixture
  2. additionby adding 200 mL of dichloromethane and 100 mL of saturated aqueous NaCl solution
  3. extractionExtract the aqueous phase with 100 mL of dichloromethane
  4. washwash them with saturated aqueous NaCl solution (100 mL)
  5. dry with materialdry them over MgSO4
  6. customcarry out drying in vacuo

出典と根拠

ORDレコード
ord-1d189e75c9634fadb2e94355772fedd2
出典データセット
uspto-grants-2014_09
特許番号
US08835627B2

反応ノート

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