Toluene → 1-Bromo-12-(4-phenylpiperazinyl)dodecane

HRID 36762

반응식

HRID 36762 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][Br:14].[C:15]1([N:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(N(CC)CC)C.C1(C)C=CC=CC=1>C(OCC)(=O)C>[Br:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][N:24]1[CH2:25][CH2:26][N:21]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH2:22][CH2:23]1

참가 물질

6

반응물 4

HCID 1140TolueneHCID 70961-PhenylpiperazineHCID 8471TriethylamineHCID 187661,12-Dibromododecane

생성물 1

HCID 199377541-Bromo-12-(4-phenylpiperazinyl)dodecane수율 50.1%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 6.56 g of 1,12-dibromododecane, 3.24 g of N-phenylpiperazine, 2.53 g of triethylamine, and 50 ml of toluene was heated under reflux for 2 hours. To the reaction mixture was added 100 ml of ethyl acetate, and the mixture was washed successively with water and a saturated sodium chloride aqueous solution, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was subjected to column chromatography using a 1:2 mixture of ethyl acetate and hexane as a developing solvent to yield 4.1 g of 1-bromo-12-(4-phenylpiperazinyl)dodecane (m.p.=26.0°-28.0° C.).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. washthe mixture was washed successively with water
  4. dry with materiala saturated sodium chloride aqueous solution, and dried over magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. additiona 1:2 mixture of ethyl acetate and hexane as a developing solvent

출처 및 근거

ORD 기록
ord-fa353175c04246a7aadabf201b983965
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05416212

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