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Hydrochloric Acid → HCID 69107963, 화합물

HRID 657657
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HRID 657657 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]2[CH:17]=[CH:16][N+:15]([O-:18])=[CH:14][CH:13]=2)=[CH:8][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].C(O)(=O)C(C1C=CC=CC=1)O.[CH3:36][C@H:37]1[CH2:42][CH2:41][CH2:40][NH:39][CH2:38]1.Cl>CN(C)C=O.C(O)C.C(N(CC)CC)C>[ClH:1].[CH3:36][C@H:37]1[CH2:42][CH2:41][CH2:40][N:39]([CH2:2][CH2:3][CH2:4][O:5][C:6]2[CH:11]=[CH:10][C:9]([C:12]3[CH:17]=[CH:16][N+:15]([O-:18])=[CH:14][CH:13]=3)=[CH:8][CH:7]=2)[CH2:38]1
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참가 물질

8

반응물 4

HCID 313Hydrochloric Acid2회HCID 11430Potassium CarbonateHCID 13929038HCID 13929038, 화합물2회HCID 23150273HCID 23150273, 화합물

생성물 1

HCID 69107963HCID 69107963, 화합물수율 23.6%

시약·촉매·용매 3

HCID 702Ethanol
용매
HCID 6228Dimethylformamide용매
HCID 8471Triethylamine용매

실험 절차

To a solution of 4-[4-(3-chloropropoxy)phenyl]pyridine 1-oxide (231 mg) and triethylamine (366 μL) in N,N-dimethylformamide (5 mL) are added potassium carbonate (363 mg) and (3S)-3-methylpiperidine mandelate (264 mg). The mixture is stirred at a temperature close to 60° C. for four hours. An additional amount of (3S)-3-methylpiperidine mandelate (100 mg) is added and heating is continued overnight. The suspension is filtered and the precipitate washed with ethyl acetate. The combined organic phases are concentrated under reduced pressure. The residue is purified twice by column chromatography over silica gel using a gradient dichloromethane/methanol/triethylamine from 100/0/0 to 95/5/0.1. Fractions containing the expected product are pooled and concentrated under reduced pressure to give 90 mg of the crude base which is converted to the hydrochloride with an ethereal solution of hydrogen chloride in ethanol to give 75 mg of (3S)-4-{4-[3-(3-methylpiperidin-1-yl)propoxy]phenyl}pyridine 1-oxide, hydrochloride melting at 74° C.

후처리

  1. customclose to 60° C. for four hours
  2. temperatureheating
  3. filtrationThe suspension is filtered
  4. washthe precipitate washed with ethyl acetate
  5. concentrationThe combined organic phases are concentrated under reduced pressure
  6. customThe residue is purified twice by column chromatography over silica gel using a gradient dichloromethane/methanol/triethylamine from 100/0/0 to 95/5/0.1
  7. additionFractions containing the expected product
  8. concentrationconcentrated under reduced pressure
  9. customto give 90 mg of the crude base which

출처 및 근거

ORD 기록
ord-2b9bce58c73449bb8f5c62a9f2b51f14
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08076329B2

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