Potassium Carbonate → 2,6-Bis-(1,1-dimethylethyl)-4-{[4-(4-nitrophenyl)-1-piperazinyl]-methyl}-phenol

HRID 987021

반응식

HRID 987021 반응식
[CH3:1][C:2]([C:5]1[CH:10]=[C:9]([CH2:11]Br)[CH:8]=[C:7]([C:13]([CH3:16])([CH3:15])[CH3:14])[C:6]=1[OH:17])([CH3:4])[CH3:3].C(=O)([O-])[O-].[K+].[K+].[N+:24]([C:27]1[CH:32]=[CH:31][C:30]([N:33]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]2)=[CH:29][CH:28]=1)([O-:26])=[O:25]>CN(C=O)C.ClCCl>[CH3:1][C:2]([C:5]1[CH:10]=[C:9]([CH2:11][N:36]2[CH2:37][CH2:38][N:33]([C:30]3[CH:29]=[CH:28][C:27]([N+:24]([O-:26])=[O:25])=[CH:32][CH:31]=3)[CH2:34][CH2:35]2)[CH:8]=[C:7]([C:13]([CH3:16])([CH3:15])[CH3:14])[C:6]=1[OH:17])([CH3:4])[CH3:3]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 804471-(4-Nitrophenyl)piperazineHCID 612973Phenol, 4-(bromomethyl)-2,6-bis(1,1-dimethylethyl)-

생성물 1

HCID 28386612,6-Bis-(1,1-dimethylethyl)-4-{[4-(4-nitrophenyl)-1-piperazinyl]-methyl}-phenol수율 54.3%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

In a 100 ml flask containing a solution of 2.99 g (10 mmoles) of 2,6-bis-(1,1-dimethylethyl)-4-bromomethylphenol in 30 ml of DMF, 1.38 g (10 mmoles) of potassium carbonate and 2.07 g (10 mmoles) of 1-(4-nitrophenyl)piperazine are added successively. After agitation for two hours at ambient temperature, the reaction medium is diluted with 150 ml of dichloromethane and washed successively with 3×40 ml of water followed by 40 ml of brine. The organic solution is dried over sodium sulphate, filtered and concentrated under reduced pressure. The brown residue obtained is purified on a silica gel column (eluant: petroleum ether (B.p. 40-70° C.)/ethyl acetate: 8/2). After concentration of the pure fractions, 2.31 g (54%) of a brown powder is obtained. Melting point: 177.5-178.5° C.

후처리

  1. additionare added successively
  2. washwashed successively with 3×40 ml of water
  3. dry with materialThe organic solution is dried over sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe brown residue obtained
  7. customis purified on a silica gel column (eluant: petroleum ether (B.p. 40-70° C.)/ethyl acetate: 8/2)

출처 및 근거

ORD 기록
ord-a0ac114d0298493cadc1b6f07edbcac3
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06630461B2

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