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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Ethyl chloroformate → Ethyl 4-(hydroxymethyl)piperidine-1-carboxylate

HRID 2106648
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반응식

HRID 2106648 반응식
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
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참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform
용매
2회

반응 조건

온도
20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6f6469db1ac847fb9c1db74b98387df3
출처 데이터셋
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04931449

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