Hydrogen Bromide → HCID 70004170, compound

HRID 580901Notes

Reaction equation

HRID 580901 reaction equation
Cl.[OH:2][C:3]1[C:8]2=[N:9][C:10]([CH3:17])=[C:11]([CH2:14][CH2:15]O)[C:12](=[O:13])[N:7]2[CH:6]=[CH:5][CH:4]=1.[BrH:18]>>[BrH:18].[Br:18][CH2:15][CH2:14][C:11]1[C:12](=[O:13])[N:7]2[CH:6]=[CH:5][CH:4]=[C:3]([OH:2])[C:8]2=[N:9][C:10]=1[CH3:17]

Participants

3

Reactant 2

HCID 260Hydrogen BromideHCID 46852369HCID 46852369, compound

Product 1

HCID 70004170HCID 70004170, compoundYield 34%

Procedure

A mixture of intermediate 9 (170 g) and hydrobromic acid (48%) (1000 ml) was stirred and refluxed overnight. The mixture was cooled and the precipitate was filtered off, yielding a first fraction of 100 g. The filtrate was evaporated, yielding a second fraction of 30 g. Both fractions were recrystallized from water, yielding 75 g (34%) of 3-(2-bromoethyl)-9-hydroxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one monohydro-bromide (intermediate 15).

Workup

  1. temperaturerefluxed overnight
  2. temperatureThe mixture was cooled
  3. filtrationthe precipitate was filtered off
  4. customyielding a first fraction of 100 g
  5. customThe filtrate was evaporated
  6. customyielding a second fraction of 30 g
  7. customBoth fractions were recrystallized from water

Sources & evidence

ORD record
ord-05092928cfbf462e85ef438032a19fdb
Source dataset
uspto-grants-1999_07
Patent number
US05919788

Reaction notes

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