Hydrogen Bromide → HCID 19830348, compound
Reaction equation
Cl.Cl.C(C1C([O:11]C)=C(OC)C=CC=1CCN[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][NH:23][CH2:24][CH2:25][C:26]1[CH:31]=[CH:30][C:29]([O:32]C)=[C:28]([O:34]C)[C:27]=1[CH2:36][CH3:37])C.[BrH:38]>>[OH2:11].[BrH:38].[BrH:38].[CH2:22]([NH:23][CH2:24][CH2:25][C:26]1[C:27]([CH2:36][CH3:37])=[C:28]([OH:34])[C:29]([OH:32])=[CH:30][CH:31]=1)[CH2:21][CH2:20][CH2:19][CH2:18][CH2:22][NH:23][CH2:24][CH2:25][C:26]1[C:27]([CH2:36][CH3:37])=[C:28]([OH:34])[C:29]([OH:32])=[CH:30][CH:31]=1Participants
3
Procedure
A suspension of Example 4 (i) (400 mg) in deoxygenated 48% hydrobromic acid (10 ml) was heated and stirred under reflux stirred for 24 h. A slow stream of nitrogen was passed through the mixture. The resulting solution was cooled and evaporated in vacuo. The solid obtained was recrystallised from methanol-ethyl acetate to give the title compound as a tan solid (300 mg), m.p. 200°-202°.
Workup
- temperatureunder reflux
- stirringstirred for 24 h
- temperatureThe resulting solution was cooled
- customevaporated in vacuo
- customThe solid obtained
- customwas recrystallised from methanol-ethyl acetate
Sources & evidence
- ORD record
- ord-59cac67aae954dcc9d94354c90afcd92
- Source dataset
- uspto-grants-1991_06
- Patent number
- US05023378
Reaction notes
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