Sodium borohydride → HCID 22767883, compound
Reaction equation
[BH4-].[Na+].[F:3][C:4]1[CH:25]=[CH:24][C:7]2[O:8][C:9]3[CH:23]=[CH:22][CH:21]=[CH:20][C:10]=3[C:11]([N:13]3[CH2:18][CH2:17][N:16]([CH3:19])[CH2:15][CH2:14]3)=[CH:12][C:6]=2[CH:5]=1>>[F:3][C:4]1[CH:25]=[CH:24][C:7]2[O:8][C:9]3[CH:23]=[CH:22][CH:21]=[CH:20][C:10]=3[CH:11]([N:13]3[CH2:18][CH2:17][N:16]([CH3:19])[CH2:15][CH2:14]3)[CH2:12][C:6]=2[CH:5]=1Participants
Procedure
6.15 g. of sodium borohydride are added in small portions over a period of 15 minutes to a solution of 12.3 g. of 1-[2-fluoro-dibenzo[b,f]oxepin-10-yl-4-methyl-piperazine in 185 ml. of glacial acid with cooling in such a manner that the temperature does not exceed 25° C. The mixture is stirred for an additional 1 hour at room temperature and the acetic acid is then evaporated in vacuo. The residue is partitioned between 3-N sodium hydroxide solution and chloroform. The aqueous phase is separated and extracted again with chloroform. The chloroform extracts are washed three times with water, dried over sodium sulfate, evaporated in vacuo, and there is obtained 1-[2-fluoro-10,11-dihydro-dibenzo [b,f]-oxepin-10-yl]-4-methyl-piperazine as a crystalline residue. The dihydrochloride, prepared in ethanol, melts at 240°-241° C. (with decomposition).
Workup
- temperatureof glacial acid with cooling in such a manner that the temperature
- customdoes not exceed 25° C
- customthe acetic acid is then evaporated in vacuo
- customThe residue is partitioned between 3-N sodium hydroxide solution and chloroform
- customThe aqueous phase is separated
- extractionextracted again with chloroform
- washThe chloroform extracts are washed three times with water
- dry with materialdried over sodium sulfate
- customevaporated in vacuo
Sources & evidence
- ORD record
- ord-2cef1a1b5ca94144889dab12b1349f40
- Source dataset
- uspto-grants-1978_05
- Patent number
- US04091023
Reaction notes
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