Water → 1-(2-Bromoacetyl)-4-(4-ethylphenoxy)piperidine

HRID 463326노트

반응식

HRID 463326 반응식
[Br:1][CH2:2][C:3](Br)=[O:4].C(=O)(O)[O-].[Na+].[CH2:11]([C:13]1[CH:25]=[CH:24][C:16]([O:17][CH:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[CH:15][CH:14]=1)[CH3:12].O>ClCCl>[Br:1][CH2:2][C:3]([N:21]1[CH2:22][CH2:23][CH:18]([O:17][C:16]2[CH:24]=[CH:25][C:13]([CH2:11][CH3:12])=[CH:14][CH:15]=2)[CH2:19][CH2:20]1)=[O:4]

참가 물질

6

반응물 4

HCID 962WaterHCID 61147Bromoacetyl bromideHCID 516892Sodium BicarbonateHCID 134574294-(4-Ethylphenoxy)piperidine

생성물 1

HCID 202831151-(2-Bromoacetyl)-4-(4-ethylphenoxy)piperidine수율 96.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a stirred suspension of 6.03 ml (69.3 mmol) of bromoacetyl bromide, 13.0 g (155 mmol) of sodium bicarbonate and 160 ml of dry dichloromethane in an ice bath was added dropwise a solution of 13.0 g (63.4 mmol) of 4-(4-ethylphenoxy)piperidine in 140 ml of dry dichloromethane. The mixture was stirred 1 hour at 0° and 45 minutes at room temperature. The mixture was subsequently poured into water, extracted twice with dichloromethane, washed with saturated sodium chloride and dried over potassium carbonate. Filtration followed by evaporation of the solvent provided 20.0 g (61.3 mmol) of 1-(2-bromoacetyl)-4-(4-ethylphenoxy)piperidine as an oil.

후처리

  1. extractionextracted twice with dichloromethane
  2. washwashed with saturated sodium chloride
  3. dry with materialdried over potassium carbonate
  4. filtrationFiltration
  5. customfollowed by evaporation of the solvent

출처 및 근거

ORD 기록
ord-e42d91b4c432488c8cdb8b11af37204e
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04518713

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