Hydrogen Bromide → HCID 19850133, compound

HRID 414390Notes

Reaction equation

HRID 414390 reaction equation
[F:1][C:2]1[CH:7]=[C:6]([CH2:8][CH2:9][NH:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][NH:17][CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:5]=[CH:4][C:3]=1[OH:26].[BrH:27]>[PH2](O)=O>[BrH:27].[BrH:27].[F:1][C:2]1[CH:7]=[C:6]([CH2:8][CH2:9][NH:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][NH:17][CH2:18][CH2:19][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:5]=[CH:4][C:3]=1[OH:26]

Participants

4

Reactant 2

HCID 260Hydrogen BromideHCID 19850134HCID 19850134, 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-867d94ca17a6452db859bbe8c9a780c0
Source dataset
uspto-grants-1988_12
Patent number
US04791216

Reaction notes

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