Water → HCID 19822588, 화합물

HRID 728624노트

반응식

HRID 728624 반응식
[CH3:1][N:2]1[CH2:20][CH:19]2[N:5]([C:6]3[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=3[CH2:12][C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=32)[CH2:4][CH2:3]1.[N:21]#CBr.O>C1C=CC=CC=1.C(OCC)C>[C:1]([N:2]1[CH2:3][CH2:4][N:5]2[C:6]3[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=3[CH2:12][C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=3[CH:19]2[CH2:20]1)#[N:21]

참가 물질

6

반응물 3

HCID 962WaterHCID 4184MianserinHCID 10476Cyanogen Bromide

생성물 1

HCID 19822588HCID 19822588, 화합물

시약·촉매·용매 2

HCID 241Benzene용매2회HCID 3283Diethyl Ether용매

실험 절차

A solution of mianserin (5.2 g) in anhydrous benzene (20 ml) was added slowly to a stirred solution of cyanogen bromide (2.3 g) in anhydrous benzene (20 ml) in an atmosphere of nitrogen. After 24 hours, the mixture was diluted with diethyl ether (50 ml) and shaken with water (50 ml). The separated aqueous layer was back extracted with a mixture of benzene and ether (equal volumes of each, total 50 ml) and the combined organic layers dried over anhydrous potassium carbonate and then evaporated under reduced pressure. The residual solid was recrystallised from ethanol to give 2-cyanonormianserin as colourless needles m.p. 164°-166° C. This compound is outside general formula I, and was used as an intermediate only.

후처리

  1. extractionThe separated aqueous layer was back extracted with a mixture of benzene and ether (equal volumes of each, total 50 ml) and the combined organic layers
  2. dry with materialdried over anhydrous potassium carbonate
  3. customevaporated under reduced pressure
  4. customThe residual solid was recrystallised from ethanol

출처 및 근거

ORD 기록
ord-3d8ff0c6c4fe498091ca8ebf9ed6013e
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05049637

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