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

HRID 35170

反応式

HRID 35170 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][CH2:19][O-:20].[Na+]>>[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:20][CH2:19][CH3:18])[CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1

参加物

3

反応物 2

HCID 2723922Sodium ethoxideHCID 198338865,7-dihydro-6H-dibenz[c,e]azepine-6carbonitrile

生成物 1

HCID 19833914ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6carboximidate

実験手順

5 g of 5,7-dihydro-6H-dibenz[c,e]azepine-6-carbonitrile in 60 ml of absolute alcohol are heated to reflux temperature for 1 hour in the presence of 30 mg of sodium ethylate. After distilling off the alcohol the residue is treated with water and the mixture is extracted three times with methylene chloride. The combined extracts are washed with water, dried over anhydrous sodium sulphate and evaporated, and the residue is distilled in a bulb-tube oven at 230°-250° C./0.1 mmHg. There is obtained ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboximidate as a clear resin which becomes solid; m.p. 68°-71° C.

後処理

  1. distillationAfter distilling off the alcohol the residue
  2. additionis treated with water
  3. extractionthe mixture is extracted three times with methylene chloride
  4. washThe combined extracts are washed with water
  5. dry with materialdried over anhydrous sodium sulphate
  6. customevaporated
  7. distillationthe residue is distilled in a bulb-tube oven at 230°-250° C./0.1 mmHg

出典と根拠

ORDレコード
ord-67d06265f1094e16befb88469c1d5334
出典データセット
uspto-grants-1988_08
特許番号
US04766115

関連ノート

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