Sodium → methyl 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboximidate

HRID 1762693노트

반응식

HRID 1762693 반응식
[CH:1]1[C:11]2[C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[CH2:8][N:7]([C:16]#[N:17])[CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[CH3:18][O-:19].[Na+].[Na]>CO>[CH:1]1[C:11]2[C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[CH2:8][N:7]([C:16](=[NH:17])[O:19][CH3:18])[CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 198338865,7-dihydro-6H-dibenz[c,e]azepine-6carbonitrile

생성물 1

HCID 19833984methyl 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboximidate

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

1.5 g of 5,7-dihydro-6H-dibenz[c,e]azepine-6-carbonitrile are added to a solution of sodium methylate in methanol prepared from 0.16 g of sodium and 20 ml of absolute methanol, and the mixture is heated to reflux temperature for 1 hour. The solvent is subsequently distilled off, the residue is treated with water and the resulting aqueous mixture is extracted three times with methylene chloride. The combined extracts are washed with water, dried over anhydrous sodium sulphate and evaporated. In this manner there is obtained methyl 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboximidate as an oil.

후처리

  1. temperaturethe mixture is heated
  2. temperatureto reflux temperature for 1 hour
  3. distillationThe solvent is subsequently distilled off
  4. additionthe residue is treated with water
  5. extractionthe resulting aqueous mixture is extracted three times with methylene chloride
  6. washThe combined extracts are washed with water
  7. dry with materialdried over anhydrous sodium sulphate
  8. customevaporated

출처 및 근거

ORD 기록
ord-a5867a16c9ce43589c4b047dca1b983b
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04833245

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