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

HRID 1881683
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HRID 1881683 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]
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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) was cooled to 0° C. Thionyl chloride (7.54 ml, 104.3 mmol) was slowly added at this temperature. The reaction mixture was heated under reflux for 12 h. The solvent was evaporated off under reduced pressure. The residue was suspended in ethyl acetate and the suspension was heated under reflux. The suspension was filtered hot. A white precipitate precipitates out in the filtrate, and was filtered out and dried under reduced pressure to give the product methyl 4-(piperidine-2-yl)butanoate hydrochloride (2) (3.49 g, 45%).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureunder reflux for 12 h
  3. customThe solvent was evaporated off under reduced pressure
  4. temperaturethe suspension was heated
  5. temperatureunder reflux
  6. filtrationThe suspension was filtered hot
  7. customA white precipitate precipitates out in the filtrate
  8. filtrationwas filtered out
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-1bfeece9c79545f4ba90cda4d6079ccd
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318769B2

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