Water → HCID 86606806, 화합물

HRID 1437629노트

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HRID 1437629 반응식
Cl.[F:2][C:3]([F:29])([F:28])[C:4]1[CH:5]=[C:6]([CH:21]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:23]=1)[CH2:7][O:8][C@H:9]1[CH2:14][CH2:13][NH:12][CH2:11][C@H:10]1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[C:30](Cl)(=[O:32])[CH3:31].O>C1COCC1.CCN(CC)CC>[C:30]([N:12]1[CH2:13][CH2:14][C@H:9]([O:8][CH2:7][C:6]2[CH:21]=[C:22]([C:24]([F:27])([F:25])[F:26])[CH:23]=[C:4]([C:3]([F:2])([F:28])[F:29])[CH:5]=2)[C@H:10]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH2:11]1)(=[O:32])[CH3:31]

참가 물질

6

반응물 3

HCID 962WaterHCID 6367Acetyl chlorideHCID 86606807cis-4-[[3,5-Bis(trifluoromethyl)benzyl]oxy]-3-phenylpiperidine hydrochloride

생성물 1

HCID 86606806HCID 86606806, 화합물수율 66%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8471Triethylamine용매

실험 절차

To a solution of the compound (0.15 g) obtained in Example 1 in THF (5.0 ml), Et3N (0.15 ml) was added, acetyl chloride (0.040 ml) was added at 0° C., and the reaction mixture was stirred at room temperature for 1 hour. The reaction mixture was poured into water, and then the product was extracted with ethyl acetate. The organic layer was washed with an aqueous 10% citric acid solution and saturated brine, dried, and then the solvent was evaporated under reduced pressure. The obtained residue was isolated and purified by silica gel column chromatography (ethyl acetate:hexane=1:1→1:0) to obtain the title compound as colorless oil (0.10 g, 66%).

후처리

  1. extractionthe product was extracted with ethyl acetate
  2. washThe organic layer was washed with an aqueous 10% citric acid solution and saturated brine
  3. customdried
  4. customthe solvent was evaporated under reduced pressure
  5. customThe obtained residue was isolated
  6. custompurified by silica gel column chromatography (ethyl acetate:hexane=1:1→1:0)

출처 및 근거

ORD 기록
ord-c76c498ba49f468ab03b095421b434e7
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07622487B2

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