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1,3-Difluoroacetone → (R)-1-(1,3-difluoropropan-2-yl)pyrrolidin-3-amine

HRID 573156
Notes
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Reaction equation

HRID 573156 reaction equation
[NH:1]1[CH2:5][CH2:4][C@@H:3]([NH:6]C(=O)OC(C)(C)C)[CH2:2]1.[F:14][CH2:15][C:16](=O)[CH2:17][F:18].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCl>[F:14][CH2:15][CH:16]([N:1]1[CH2:5][CH2:4][C@@H:3]([NH2:6])[CH2:2]1)[CH2:17][F:18]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 2283971,3-DifluoroacetoneHCID 1514397(3R)-(+)-3-(tert-Butoxycarbonylamino)pyrrolidineHCID 5049666Sodium triacetoxyborohydride

Product 1

HCID 67126443(R)-1-(1,3-difluoropropan-2-yl)pyrrolidin-3-amine

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of (R)-tert-butyl pyrrolidin-3-ylcarbamate (0.500 g) and 1,3-difluoropropan-2-one (0.278 g) in dichloromethane (5 mL) was added sodium triacetoxyborohydride (0.853 g). After stirring for 1 hour, the reaction was quenched with saturated NaHCO3 solution (5 mL). The product was extracted into dichloromethane (25 mL), dried over magnesium sulfate, filtered, and concentrated. The resulting crude material was treated with HCl (4.0M in dioxane, 4 mL) and methanol (1 mL) and stirred for 1 hour. The mixture was concentrated to provide the title compound.

Workup

  1. customthe reaction was quenched with saturated NaHCO3 solution (5 mL)
  2. extractionThe product was extracted into dichloromethane (25 mL)
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. additionThe resulting crude material was treated with HCl (4.0M in dioxane, 4 mL) and methanol (1 mL)
  7. stirringstirred for 1 hour
  8. concentrationThe mixture was concentrated

Sources & evidence

ORD record
ord-82df88e44f3a48f0965fc62a96934ead
Source dataset
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09029404B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes