Hydrogen Bromide → HCID 19850133, compound

HRID 542543Notes

Reaction equation

HRID 542543 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°-242°-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°-242°-5°

Sources & evidence

ORD record
ord-c39343be70bb4d9f8fc45b5678f9050b
Source dataset
uspto-grants-1987_04
Patent number
US04657929

Reaction notes

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