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

HRID 1762693ノート

反応式

HRID 1762693 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a5867a16c9ce43589c4b047dca1b983b
出典データセット
uspto-grants-1989_05
特許番号
US04833245

反応ノート

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