Mianserin → HCID 19261489、化合物

HRID 2225372ノート

反応式

HRID 2225372 の反応式
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].C[N:8]1[CH2:26][CH2:25][N:11]2[C:12]3[CH:24]=[CH:23][CH:22]=[CH:21][C:13]=3[CH2:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[CH:10]2[CH2:9]1.C(=O)(O)[O-].[Na+]>C1C=CC=CC=1>[CH2:9]1[CH:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][C:13]3[CH:21]=[CH:22][CH:23]=[CH:24][C:12]=3[N:11]2[CH2:25][CH2:26][N:8]1[C:2]([O:4][CH2:5][CH3:6])=[O:3]

参加物

5

反応物 3

HCID 4184MianserinHCID 10928Ethyl chloroformateHCID 516892Sodium Bicarbonate

生成物 1

HCID 19261489HCID 19261489、化合物収率 74.9%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

Ethyl chloroformate (19.53 g) was added dropwisely to a solution of 9.52 g of 1,2,3,4,10,14b-hexahydro-2-methyldibenzo[c,f]pyrazino[1,2-a]azepine in 48 ml of benzene at refluxed temperature and the mixture was refluxed for 5 hrs. Ice water was added to the reaction mixture and made alkaline with sodium bicarbonate. The mixture was extracted with benzene and the benzene layer was washed with water, dried and concentrated. The residue was chromatographed on silica gel using a mixture of n-hexane and ethyl acetate as an eluent (1:2) to give 8.70 g of pale yellow crystals, which were recrystallized from a mixture of isopropyl ether and n-pentane to give pale yellow prisms, mp 108.5°-109.5° C.

後処理

  1. temperatureat refluxed temperature
  2. temperaturethe mixture was refluxed for 5 hrs
  3. extractionThe mixture was extracted with benzene
  4. washthe benzene layer was washed with water
  5. customdried
  6. concentrationconcentrated
  7. customThe residue was chromatographed on silica gel using
  8. additiona mixture of n-hexane and ethyl acetate as an eluent (1:2)

出典と根拠

ORDレコード
ord-4400666a1002444ea2bfe96edc378366
出典データセット
uspto-grants-1994_09
特許番号
US05344828

反応ノート

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