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2-Methylpiperidine → 2-Methyl-1-(2-propynyl)piperidine

HRID 1808695
ノート
印刷プレビュー

反応式

HRID 1808695 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 79742-MethylpiperidineHCID 122213-Chloro-1-propyne

生成物 1

HCID 5789632-Methyl-1-(2-propynyl)piperidine収率 22.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-de45382a5a8c4d779eb0f2e7eb1aae8d
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08361962B2

反応ノート

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