Phosphorus tribromide → HCID 178429162, compound

HRID 1755921Notes

Reaction equation

HRID 1755921 reaction equation
O[CH2:2][C:3]1[N:13]=[C:6]2[NH:7][C:8]([CH3:12])=[CH:9][C:10](=[O:11])[N:5]2[N:4]=1.P(Br)(Br)[Br:15]>CN(C)C=O>[Br:15][CH2:2][C:3]1[N:13]=[C:6]2[N:7]=[C:8]([CH3:12])[CH:9]=[C:10]([OH:11])[N:5]2[N:4]=1

Participants

4

Reactant 2

HCID 24614Phosphorus tribromideHCID 178429175HCID 178429175, compound

Product 1

HCID 178429162HCID 178429162, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

2-(Hydroxymethyl)-5-methyl-s-triazolo[1,5-a]pyrimidin-7(4H)-one (U.S. Pat. No. 2,835,581) (1.8 g) is suspended in 5 ml of dimethylformamide, treated with 0.45 ml of phosphorus tribromide at 0° C. and stirred at this temperature for 1/2 hour. The dimethylformamide is evaporated in a high vacuum and the residue is digested with ice-cold water. The resulting precipitate is filtered off under suction and dried in a high vacuum (40° C.). There are obtained 1.97 g of 2-bromomethyl-5-methyl[1.2.4]triazolo[1,5-a]pyrimidin-7-ol as white crystals of melting point 217°-222° C.

Workup

  1. customThe dimethylformamide is evaporated in a high vacuum
  2. filtrationThe resulting precipitate is filtered off under suction
  3. customdried in a high vacuum (40° C.)

Sources & evidence

ORD record
ord-c8a7393c0f8442ddbf4c399085eeeba8
Source dataset
uspto-grants-1995_08
Patent number
US05438052

Reaction notes

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