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

HRID 35173

반응식

HRID 35173 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ec01c07dd42e42d19e85933e8284aee8
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766115

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