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

HRID 76325노트

반응식

HRID 76325 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1d189e75c9634fadb2e94355772fedd2
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835627B2

반응 노트

불러오는 중…