1,4-Bis(bromomethyl)benzene → HCID 20322504, 화합물

HRID 840007노트

반응식

HRID 840007 반응식
[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]

참가 물질

5

반응물 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

생성물 1

HCID 20322504HCID 20322504, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fda41a52a5664b799f8d905c778db651
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04097587

반응 노트

불러오는 중…