1,4-Bis(bromomethyl)benzene → HCID 20322504、化合物

HRID 840007ノート

反応式

HRID 840007 の反応式
[K].[CH2:2]([C:4]1([CH3:20])[NH:15][C:14]([CH2:17][CH3:18])([CH3:16])[CH2:13][C:6]2([NH:10][C:9](=[O:11])[NH:8][C:7]2=[O:12])[CH:5]1[CH3:19])[CH3:3].Br[CH2:22][C:23]1[CH:28]=[CH:27][C:26]([CH2:29]Br)=[CH:25][CH:24]=1>CN(C)C=O>[CH2:2]([C:4]1([CH3:20])[NH:15][C:14]([CH2:17][CH3:18])([CH3:16])[CH2:13][C:6]2([NH:10][C:9](=[O:11])[N:8]([CH2:22][C:23]3[CH:28]=[CH:27][C:26]([CH2:29][N:8]4[C:7](=[O:12])[C:6]5([CH2:13][C:14]([CH3:16])([CH2:17][CH3:18])[NH:15][C:4]([CH3:20])([CH2:2][CH3:3])[CH:5]5[CH3:19])[NH:10][C:9]4=[O:11])=[CH:25][CH:24]=3)[C:7]2=[O:12])[CH:5]1[CH3:19])[CH3:3]

参加物

5

反応物 3

HCID 693351,4-Bis(bromomethyl)benzeneHCID 5462222PotassiumHCID 203401897,9-Diethyl-6,7,9-trimethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione

生成物 1

HCID 20322504HCID 20322504、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

To 80 ml of dimethylformamide were added 8.0 g of the potassium salt of 7,9-diethyl-6,7,9-trimethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione and 3.1 g of α,α'-dibromo-p-xylene; the mixture was heated, with stirring, at 60° C for 3 hours. The mixture was then concentrated by evaporation under reduced pressure and the residue was dissolved in chloroform. The chloroform solution was washed with water and dried over magnesium sulphate; the chloroform was then removed. The residue was purified first by column chromatography on silica gel (eluent: a 6 : 3 : 0.5 by volume mixture of ethyl acetate, benzene and triethylamine) and then by recrystallization from ethanol, giving 5.0 g of Compound 43 as crystals melting at 272° - 274° C.

後処理

  1. temperaturethe mixture was heated
  2. concentrationThe mixture was then concentrated by evaporation under reduced pressure
  3. dissolutionthe residue was dissolved in chloroform
  4. washThe chloroform solution was washed with water
  5. dry with materialdried over magnesium sulphate
  6. customthe chloroform was then removed
  7. customThe residue was purified first by column chromatography on silica gel (eluent
  8. additiona 6 : 3 : 0.5 by volume mixture of ethyl acetate, benzene and triethylamine) and then
  9. customby recrystallization from ethanol

出典と根拠

ORDレコード
ord-fda41a52a5664b799f8d905c778db651
出典データセット
uspto-grants-1978_06
特許番号
US04097587

反応ノート

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