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

HRID 36762

反応式

HRID 36762 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 199377541-Bromo-12-(4-phenylpiperazinyl)dodecane収率 50.1%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-fa353175c04246a7aadabf201b983965
出典データセット
uspto-grants-1995_05
特許番号
US05416212

関連ノート

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