Hydrochloric Acid → HCID 18357661, compound
Reaction equation
N1([C:6]23[CH2:21][CH2:20][CH2:19][CH2:18][CH:7]2[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Br:17])=[N:9][O:10]3)CCCC1.Cl.[OH-].[K+]>CO>[O:10]1[C:6]2[CH2:21][CH2:20][CH2:19][CH2:18][C:7]=2[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Br:17])=[N:9]1Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
To a stirred solution of 5.8 g of 2-(3a,4,5,6,7,7a-hexahydro-7a-pyrrolidino1,2-benzisoxazol-3-yl)-bromobenzene in 60 ml of methanol was added 100 ml of concentrated hydrochloric acid and the solution was refluxed for 20 min. The solution was cooled to room temperature and neutralised with 10M potassium hydroxide solution. The solution was extracted with 400 ml then 200 ml of methylene chloride and the combined organic layers were dried over sodium sulfate and evaporated to yield 4.5 g of 2-(4,5,6,7-tetrahydro1,2-benzisoxazol-3-yl)-bromobenzene as a gum, GC-M.S. (E.I.) (MIZ): 277 [M]+.
Workup
- temperaturethe solution was refluxed for 20 min
- extractionThe solution was extracted with 400 ml
- dry with material200 ml of methylene chloride and the combined organic layers were dried over sodium sulfate
- customevaporated
Sources & evidence
- ORD record
- ord-42630713edd24c39bb00d70158a7b361
- Source dataset
- uspto-grants-2000_06
- Patent number
- US06080773
Reaction notes
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