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Ethyl chloroformate → Ethyl 4-(hydroxymethyl)piperidine-1-carboxylate

HRID 2106648
ノート
印刷プレビュー

反応式

HRID 2106648 の反応式
C(=O)([O-])[O-].[K+].[K+].Cl.[NH:8]1[CH2:13][CH2:12][CH:11]([CH2:14][OH:15])[CH2:10][CH2:9]1.Cl[C:17]([O:19][CH2:20][CH3:21])=[O:18]>C(Cl)(Cl)Cl.O>[OH:15][CH2:14][CH:11]1[CH2:12][CH2:13][N:8]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:9][CH2:10]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10928Ethyl chloroformateHCID 11430Potassium CarbonateHCID 24191744(Piperidin-4-yl)methanol--hydrogen chloride (1/1)

生成物 1

HCID 19773576Ethyl 4-(hydroxymethyl)piperidine-1-carboxylate収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform
溶媒
2 回

反応条件

温度
20 °C

実験手順

168.3 g (1.22 mol) of potassium carbonate are added to a solution of 61.6 g (406 mmol) of 4-piperidinemethanol hydrochloride in a mixture of 406 ml of chloroform and 406 ml of water, followed by 42.55 ml (440 mmol) of ethyl chloroformate dissolved in 160 ml of chloroform. The mixture is stirred for 3 h at 20° C., the organic phase is separated off, the aqueous phase is extracted with dichloromethane, the organic phases are combined to form a single phase, washed with water and dried over magnesium sulphate, and the solvents are evaporated off under reduced pressure. 76 g of an oil is obtained, this being used without further treatment in the following stage.

後処理

  1. customthe organic phase is separated off
  2. extractionthe aqueous phase is extracted with dichloromethane
  3. customto form a single phase
  4. washwashed with water
  5. dry with materialdried over magnesium sulphate
  6. customthe solvents are evaporated off under reduced pressure

出典と根拠

ORDレコード
ord-6f6469db1ac847fb9c1db74b98387df3
出典データセット
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04931449

反応ノート

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