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Potassium Hydroxide → (3S)-1-(6-methoxypyridin-2-yl)pyrrolidin-3-ol

HRID 1054903
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HRID 1054903 반응식
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([O:8][CH3:9])[N:3]=1.[NH:10]1[CH2:14][CH2:13][C@H:12]([OH:15])[CH2:11]1.[OH-].[K+]>O1CCCC1.CO.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].CC(P(C(C)(C)C)C1N(C2C(C3C=CC=CC=3)=NN(C3C=CC=CC=3)C=2C2C=CC=CC=2)N=CC=1)(C)C>[CH3:9][O:8][C:4]1[N:3]=[C:2]([N:10]2[CH2:14][CH2:13][C@H:12]([OH:15])[CH2:11]2)[CH:7]=[CH:6][CH:5]=1
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참가 물질

7

반응물 3

HCID 14797Potassium HydroxideHCID 870092-Chloro-6-methoxypyridineHCID 2733874(3S)-pyrrolidin-3-ol

생성물 1

HCID 86698868(3S)-1-(6-methoxypyridin-2-yl)pyrrolidin-3-ol수율 226.5%

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium촉매
HCID 11547931
BippyPhos
촉매
HCID 21899815MeOH tetrahydrofuran용매

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온도
70 °C

실험 절차

To a solution of 2-chloro-6-methoxypyridine (1.966 g, 3.750 mmol) and commercially available (3S)-pyrrolidin-3-ol (1.437 g, 16.50 mmol) in tetrahydrofuran/methanol (137 mL/6.7 mL), was added Pd2(dba)3 (62.2 mg, 0.0688 mmol), BippyPhos (139.2 mg, 0.2750 mmol) and potassium hydroxide (1.16 g, 20.6 mmol, 88% pellets). The reaction was then was purged with nitrogen for 2 minutes and stirred at 70° C. for 18 hours. The reaction was filtered, quenched with saturated ammonium chloride solution, adjusted to pH=7˜8 with 1N hydrochloric acid and extracted with dichloromethane (100 mL*2) and ethyl acetate (100 mL*3). The combined organic phase was washed with saturated brine, dried over sodium sulfate and evaporated in vacuo. The residue was then purified by silica gel chromatography with ethyl acetate/petroleum ether, 0-25% to give the title compound (1.65 g, 62%) as a yellow gum that was used without further purification.

후처리

  1. customThe reaction was then was purged with nitrogen for 2 minutes
  2. filtrationThe reaction was filtered
  3. customquenched with saturated ammonium chloride solution
  4. extractionextracted with dichloromethane (100 mL*2) and ethyl acetate (100 mL*3)
  5. washThe combined organic phase was washed with saturated brine
  6. dry with materialdried over sodium sulfate
  7. customevaporated in vacuo
  8. customThe residue was then purified by silica gel chromatography with ethyl acetate/petroleum ether, 0-25%

출처 및 근거

ORD 기록
ord-c5dca06560d34764ae9904bdc4c3fff1
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394285B2

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