Ethyl Bromide → 1-Ethyl-4-(3-fluorobenzyl)piperidine

HRID 928046노트

반응식

HRID 928046 반응식
Br[CH2:2][CH3:3].[F:4][C:5]1[CH:6]=[C:7]([CH:15]=[CH:16][CH:17]=1)[CH2:8][CH:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:2]([N:12]1[CH2:13][CH2:14][CH:9]([CH2:8][C:7]2[CH:15]=[CH:16][CH:17]=[C:5]([F:4])[CH:6]=2)[CH2:10][CH2:11]1)[CH3:3]

참가 물질

5

반응물 3

HCID 6332Ethyl BromideHCID 11430Potassium CarbonateHCID 107281414-[(3-Fluorophenyl)methyl]piperidine2회

생성물 1

HCID 709836871-Ethyl-4-(3-fluorobenzyl)piperidine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Bromoethane (0.1 mL) was added to a mixture of 4-(3-fluorobenzyl)piperidine (Intermediate 180, 0.259 g) and potassium carbonate (0.204 g) in acetonitrile (10 mL). The mixture was stirred for 20 hours then filtered. The filtrate acidified by addition of few drops of 2M HCl and the solution was passed through a SCX-2 column (10 g). The product was eluted with 2M ammonia in methanol and the residue after evaporation was triturated with diethyl ether. The solid was filtered off and the filtrated was concentrated in vacuo to give 1-ethyl-4-(3-fluorobenzyl)piperidine (0.210 g)

후처리

  1. filtrationthen filtered
  2. additionThe filtrate acidified by addition of few drops of 2M HCl
  3. washThe product was eluted with 2M ammonia in methanol
  4. customthe residue after evaporation
  5. customwas triturated with diethyl ether
  6. filtrationThe solid was filtered off
  7. concentrationthe filtrated was concentrated in vacuo

출처 및 근거

ORD 기록
ord-9831bd9934d44785b9a1154d29da9e4c
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09290472B2

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