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Azetidine → 5-(Azetidin-1-ylmethyl)-1-methyl-3-nitro-1H-pyrazole

HRID 1431166
Notes
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Reaction equation

HRID 1431166 reaction equation
Br[CH2:2][C:3]1[N:7]([CH3:8])[N:6]=[C:5]([N+:9]([O-:11])=[O:10])[CH:4]=1.[NH:12]1[CH2:15][CH2:14][CH2:13]1.C(N(C(C)C)CC)(C)C>O1CCCC1>[N:12]1([CH2:2][C:3]2[N:7]([CH3:8])[N:6]=[C:5]([N+:9]([O-:11])=[O:10])[CH:4]=2)[CH2:15][CH2:14][CH2:13]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 10422AzetidineHCID 81531DiisopropylethylamineHCID 585403565-(Bromomethyl)-1-methyl-3-nitro-1H-pyrazole

Product 1

HCID 585403155-(Azetidin-1-ylmethyl)-1-methyl-3-nitro-1H-pyrazoleYield 90%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a solution of 5-(bromomethyl)-1-methyl-3-nitro-1H-pyrazole (436 mg, 1.98 mmol) in tetrahydrofuran (10 mL) was added azetidine (141 mg, 0.17 mL, 2.48 mmol) and diisopropylethyl amine (307 mg, 0.42 mL, 2.38 mmol) drop wise and the resulting mixture was stirred at room temperature for 24 h. The solution was concentrated and the residue dissolved in dichloromethane (50 mL), washed with water (50 mL). The aqueous layer was extracted with methylene chloride (2×50 mL) and the organic phases combined and dried over magnesium sulfate. The resulting mixture was filtered and evaporated and the residue purified by flash chromatography (40 g, 1% to 5% methanol in dichloromethane) to give 5-(azetidin-1-ylmethyl)-1-methyl-3-nitro-1H-pyrazole (349 mg, 90%) as a colorless oil.

Workup

  1. concentrationThe solution was concentrated
  2. dissolutionthe residue dissolved in dichloromethane (50 mL)
  3. washwashed with water (50 mL)
  4. extractionThe aqueous layer was extracted with methylene chloride (2×50 mL)
  5. dry with materialdried over magnesium sulfate
  6. filtrationThe resulting mixture was filtered
  7. customevaporated
  8. customthe residue purified by flash chromatography (40 g, 1% to 5% methanol in dichloromethane)

Sources & evidence

ORD record
ord-903146ff46f843d4bb222f9e5d3bfbdb
Source dataset
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08940741B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes