Hydrochloric Acid → N-(2-methoxyphenyl)piperidin-4-amine

HRID 1784702노트

반응식

HRID 1784702 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[O:21][CH3:22])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>CO.C(OCC)(=O)C>[CH3:22][O:21][C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=1[NH:14][CH:11]1[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 22557919tert-Butyl 4-((2-methoxyphenyl)amino)piperidine-1-carboxylate

생성물 1

HCID 10584422N-(2-methoxyphenyl)piperidin-4-amine수율 99%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 4-(2-methoxyphenylamino)-piperidine-1-carboxylic acid tert-butyl ester (2.7 g, 8.8 mmol) in methanol (30 mL) was added 4N hydrochloric acid in ethyl acetate (20 mL) at room temperature. After stirring for 1 h, the resulting suspension was concentrated in vacuo. The residue was partitioned between chloroform and 1N sodium hydroxide. The aqueous layer was extracted with chloroform. The combined organic layer was washed with brine, dried over magnesium sulfate, and concentrated in vacuo. The residue was purified by silica gel chromatography eluting 10-20% methanol in chloroform to furnish 4-(2-methoxyphenylamino)-piperidine (1.8 g, 8.7 mmol, 99%) as white crystals.

후처리

  1. concentrationthe resulting suspension was concentrated in vacuo
  2. customThe residue was partitioned between chloroform and 1N sodium hydroxide
  3. extractionThe aqueous layer was extracted with chloroform
  4. washThe combined organic layer was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by silica gel chromatography
  8. washeluting 10-20% methanol in chloroform

출처 및 근거

ORD 기록
ord-0ecb189bad7f45de80b6db393d2d5e90
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07504411B2

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