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

HRID 1762710

反応式

HRID 1762710 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

反応物 2

HCID 10476Cyanogen BromideHCID 811835H-Dibenz(c,e)azepine, 6,7-dihydro-

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

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-5679784e42884e2e8dcffd5a0a8d5d0f
出典データセット
uspto-grants-1989_05
特許番号
US04833245

関連ノート

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