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Sodium borohydride → 1-Cyclopropylpiperidin-4-ol

HRID 854245
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HRID 854245 반응식
[CH:1]1([N:4]2[CH2:9][CH2:8][C:7](=[O:10])[CH2:6][CH2:5]2)[CH2:3][CH2:2]1.[BH4-].[Na+]>C(O)C>[CH:1]1([N:4]2[CH2:9][CH2:8][CH:7]([OH:10])[CH2:6][CH2:5]2)[CH2:3][CH2:2]1
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참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 162276291-Cyclopropylpiperidin-4-one

생성물 1

HCID 515828091-Cyclopropylpiperidin-4-ol수율 95%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a cold (0° C.) solution of 1-cyclopropyl-piperidin-4-one (1.5 g, 11 mmol, 1.0 eq.) in absolute ethanol was added sodium borohydride (306 mg, 8 mmol, 0.75 eq.). The reaction mixture was stirred at room temperature for 65 h. The mixture was concentrated in vacuo. Ice water (10 mL) was added, followed by an aqueous solution of sodium hydroxide (28% w/w, ca. 10 mL) and dichloromethane (20 mL). The mixture was stirred at room temperature for 2 h. After phase separation, the aqueous layer was extracted with dichloromethane. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and evaporated in vacuo. The crude mixture was purified on silica eluting with DCM/2N NH3 in methanol 93/7, yielding to 1.44 g (95%) of the desired product as a colorless oil. MS (m/e): 423.1 (MH+, 100%)

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. additionIce water (10 mL) was added
  3. stirringThe mixture was stirred at room temperature for 2 h
  4. customAfter phase separation
  5. extractionthe aqueous layer was extracted with dichloromethane
  6. washThe combined organic layers were washed with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. customevaporated in vacuo
  10. customThe crude mixture was purified on silica eluting with DCM/2N NH3 in methanol 93/7

출처 및 근거

ORD 기록
ord-2b30dc9373c2443b9dc1c2b34430c500
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07259158B2

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