Water → HCID 19822588、化合物

HRID 728624ノート

反応式

HRID 728624 の反応式
[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]

参加物

6

反応物 3

HCID 962WaterHCID 4184MianserinHCID 10476Cyanogen Bromide

生成物 1

HCID 19822588HCID 19822588、化合物

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3d8ff0c6c4fe498091ca8ebf9ed6013e
出典データセット
uspto-grants-1991_09
特許番号
US05049637

反応ノート

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