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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2-Methylpiperidine → 2-Methyl-1-(2-propynyl)piperidine

HRID 1808695
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HRID 1808695 반응식
[CH2:1](Cl)[C:2]#[CH:3].[CH3:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][NH:7]1>CO>[CH3:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][N:7]1[CH2:3][C:2]#[CH:1]
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참가 물질

4

반응물 2

HCID 79742-MethylpiperidineHCID 122213-Chloro-1-propyne

생성물 1

HCID 5789632-Methyl-1-(2-propynyl)piperidine수율 22.7%

시약·촉매·용매 1

HCID 887Methanol용매3회

실험 절차

A flask was charged with propargyl chloride (17.27 g, 0.232 mol, 70 wt % in toluene) in dry methanol (21 mL) under nitrogen atmosphere. (+/−)-2-Methyl-piperidine (55 mL, 0.46 mol) in dry methanol (43 mL) was added via drop-wise addition over 30 minutes. The material was stirred overnight. The mixture was placed on a rotovap and about half the volume of methanol was stripped, providing a precipitate. The solid precipitate was removed by filtration, rinsing through with ether (150 mL). The filtrite was placed on the rotovap and concentrated. Another small amount of precipitate was removed by filtration. The remaining oily product was purified by distillation providing 7.23 g (bp=180-185° C.) of (+/−)-2-methyl-1-prop-2-ynyl-piperidine as a clear mobile oil.

후처리

  1. customproviding a precipitate
  2. customThe solid precipitate was removed by filtration
  3. washrinsing through with ether (150 mL)
  4. concentrationconcentrated
  5. customAnother small amount of precipitate was removed by filtration
  6. distillationThe remaining oily product was purified by distillation

출처 및 근거

ORD 기록
ord-de45382a5a8c4d779eb0f2e7eb1aae8d
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08361962B2

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