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Sodium borohydride → 1-Cyclopropylpiperidin-4-ol

HRID 901105
Notes
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Reaction equation

HRID 901105 reaction equation
[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
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 4311764Sodium borohydrideHCID 162276291-Cyclopropylpiperidin-4-one

Product 1

HCID 515828091-Cyclopropylpiperidin-4-olYield 95%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

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%)

Workup

  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

Sources & evidence

ORD record
ord-50abefe15ada423b8b399bd0d830cded
Source dataset
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07361682B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes