Hydrogen Bromide → HCID 19850133, compound

HRID 1608010Notes

Reaction equation

HRID 1608010 reaction equation
Cl.Cl.[F:3][C:4]1[CH:5]=[C:6]([CH2:12][CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][NH:21][CH2:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:7]=[CH:8][C:9]=1[O:10]C.[BrH:30]>[PH2](O)=O>[BrH:30].[BrH:30].[F:3][C:4]1[CH:5]=[C:6]([CH2:12][CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][NH:21][CH2:22][CH2:23][C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[CH:7]=[CH:8][C:9]=1[OH:10]

Participants

4

Reactant 2

HCID 260Hydrogen BromideHCID 19850140HCID 19850140, compound

Product 1

HCID 19850133HCID 19850133, compound

Reagents, catalysts & solvents 1

HCID 4124402Phosphinic AcidCatalyst

Procedure

The product from step (b) (1.8 g) in 48% hydrobromic acid (18 ml) containing hypophosphorous acid (10 drops) was boiled at reflux under nitrogen for 5.5 hr. The solid which separated on cooling the solution was collected and recrystallised from water giving the dihydrobromide salt of the title compound as colourless needles (1.3 g) mp 240.5-142°-5°.

Workup

  1. temperatureat reflux under nitrogen for 5.5 hr
  2. customThe solid which separated
  3. temperatureon cooling the solution
  4. customwas collected
  5. customrecrystallised from water giving the dihydrobromide salt of the title compound as colourless needles (1.3 g) mp 240.5-142°-5°

Sources & evidence

ORD record
ord-78bf1d0580234c5da4a121c0d370a381
Source dataset
uspto-grants-1989_09
Patent number
US04868306

Reaction notes

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