Hydrochloric Acid → 2-[3-(3,4-Dichlorophenyl)piperidin-3-yl]ethanol

HRID 1080662노트

반응식

HRID 1080662 반응식
Cl.O1CCCCC1[O:8][CH2:9][CH2:10][C:11]1([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[C:19]([Cl:24])[CH:18]=2)[CH2:16][CH2:15][CH2:14][NH:13][CH2:12]1>CCOCC.CO.C(OC(C)C)(C)C.CCOCC>[OH:8][CH2:9][CH2:10][C:11]1([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[C:19]([Cl:24])[CH:18]=2)[CH2:16][CH2:15][CH2:14][NH:13][CH2:12]1

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 211976913-(2-Tetrahydropyranyloxyethyl)-3-(3,4-dichlorophenyl)piperidine

생성물 1

HCID 154604002-[3-(3,4-Dichlorophenyl)piperidin-3-yl]ethanol수율 106.9%

시약·촉매·용매 3

HCID 887Methanol용매HCID 3283Diethyl Ether용매HCID 21919906Ether isopropyl ether용매

실험 절차

A saturated solution of hydrogen chloride in ether is added to a solution of 55 g of 3-(2-tetrahydropyranyloxyethyl)-3-(3,4-dichlorophenyl)piperidine in 200 ml of methanol until the pH is 1. The mixture is stirred for half an hour at room temperature and concentrated to dryness, the residue is taken up in water, rendered alkaline with a solution of NaOH and extracted with CH2Cl2 and the extract is washed with a saturated solution of NaCl, dried over Na2SO4 and evaporated to dryness to give an oil. This oil is taken up in 200 ml of an isopropyl ether/ether mixture (50/50 v/v). After stirring and filtration, the product is washed with ethyl ether and dried under vacuum over P2O5 to give 45 g of the expected product. M.p.=122° C.

후처리

  1. concentrationconcentrated to dryness
  2. extractionextracted with CH2Cl2
  3. washthe extract is washed with a saturated solution of NaCl
  4. dry with materialdried over Na2SO4
  5. customevaporated to dryness
  6. customto give an oil
  7. stirringAfter stirring
  8. filtrationfiltration
  9. washthe product is washed with ethyl ether
  10. dry with materialdried under vacuum over P2O5

출처 및 근거

ORD 기록
ord-e8b61c0e4f1a4458a73ef0595584a488
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05583134

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