Cyanogen Bromide → 5,7-dihydro-6H-dibenz[c,e]azepine-6carbonitrile

HRID 35173

反応式

HRID 35173 の反応式
[N:1]#[C:2]Br.[CH:4]1[C:14]2[C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[CH2:11][NH:10][CH2:9][C:8]=2[CH:7]=[CH:6][CH:5]=1>C(Cl)(Cl)Cl>[CH:4]1[C:14]2[C:13]3[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=3[CH2:11][N:10]([C:2]#[N:1])[CH2:9][C:8]=2[CH:7]=[CH:6][CH:5]=1

参加物

4

実験手順

A solution of 1.91 g of cyanogen bromide in 20 ml of chloroform is added dropwise at 5°-10° C. within 25 minutes to a solution, cooled to 5° C., of 7 g of 6,7-dihydro-5H-dibenz[c,e]azepine in 50 ml of chloroform. The reaction mixture is stirred for a further 1 hour and then a small amount of the hydrobromide salt of the still unreacted azepine is filtered off. The filtrate is washed three times with water, dried over anhydrous sodium sulphate and evaporated. There is obtained solid 5,7-dihydro-6H-dibenz[c,e]azepine-6-carbonitrile, m.p. 123°-126° C.

後処理

  1. filtrationa small amount of the hydrobromide salt of the still unreacted azepine is filtered off
  2. washThe filtrate is washed three times with water
  3. dry with materialdried over anhydrous sodium sulphate
  4. customevaporated

出典と根拠

ORDレコード
ord-ec01c07dd42e42d19e85933e8284aee8
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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