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Methanol → Methyl 4-(piperidin-2-yl)butanoate hydrochloride

HRID 2388714
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반응식

HRID 2388714 반응식
Cl.[NH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12].S(Cl)([Cl:16])=O.[CH3:18]O>>[ClH:16].[NH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][CH2:9][CH2:10][C:11]([O:13][CH3:18])=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 124163274-(Piperidin-2-yl)butanoic acid--hydrogen chloride (1/1)

생성물 1

HCID 66772062Methyl 4-(piperidin-2-yl)butanoate hydrochloride수율 45%

실험 절차

A solution of 4-(2-piperidinyl)butanoic acid hydrochloride (5.95 g, 34.8 mmol) in Methanol (104 ml) is cooled to 0° C. At this temperature thionylchloride (7.54 ml, 104.3 mmol) is added slowly. The reaction mixture is heated to reflux for 12 h. The solvent is evaporated in vacuum. The residue is suspended in ethylacetate and is heated to reflux. The suspension is filtered while it is still hot. In the filtrate a white solid dropped out, which was filtered out and dried in vacuum to give Methyl 4-(piperidin-2-yl)butanoate hydrochloride (2) (3.49 g, 45%)

후처리

  1. temperatureThe reaction mixture is heated
  2. temperatureto reflux for 12 h
  3. customThe solvent is evaporated in vacuum
  4. temperatureis heated to reflux
  5. filtrationThe suspension is filtered while it
  6. additionIn the filtrate a white solid dropped out
  7. filtrationwhich was filtered out
  8. customdried in vacuum

출처 및 근거

ORD 기록
ord-ad4ac774d20e456bbb3b96e11797832c
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268814B2

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