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Phosphorus tribromide → 2-Propylthiazol-5-amine

HRID 607139
Notes
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Reaction equation

HRID 607139 reaction equation
[C:1]([NH:6][CH2:7][C:8]([NH2:10])=O)(=[S:5])[CH2:2][CH2:3][CH3:4].P(Br)(Br)Br>C(OCC)(=O)C>[CH2:2]([C:1]1[S:5][C:8]([NH2:10])=[CH:7][N:6]=1)[CH2:3][CH3:4]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 24614Phosphorus tribromide2×HCID 866146222-Thiobutyrylamino-acetamide

Product 1

HCID 451217592-Propylthiazol-5-amine

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

A solution of the product of Example 5C (395 mg, 2.465 mmol) in anhydrous ethyl acetate (12 mL) was treated with phosphorous tribromide (0.189 mL, 1.972 mmol) under a nitrogen atmosphere and stirred at room temperature for 20 minutes. Added additional phosphorous tribromide (0.050 mL) and let stir for 5 minutes. The reaction mixture was diluted with ethyl acetate (50 mL) and washed with saturated aqueous sodium bicarbonate (25 mL). The aqueous wash was extracted with ethyl acetate (2×50 mL), and the organic extracts were combined and washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated under vacuum giving the title compound. Purification by silica gel flash chromatography with 3% methanol/methylene afforded the title product (175 mg, 1.23 mmol, 50%).

Workup

  1. stirringlet stir for 5 minutes
  2. washwashed with saturated aqueous sodium bicarbonate (25 mL)
  3. washThe aqueous wash
  4. extractionwas extracted with ethyl acetate (2×50 mL)
  5. washwashed with brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under vacuum

Sources & evidence

ORD record
ord-5702a827e8f24c159de73b4f955a732a
Source dataset
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07915411B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes