Sodium Bicarbonate → HCID 178481966, compound
Reaction equation
[Cl-].[Cl:2][C:3]1[C:4](CC)=[CH:5][C:6]2[N:12]3[C:13]([NH:19][CH3:20])=[NH+:14][N:15]([CH2:16]CC)[CH:11]3[CH:10](C)[N:9]=[C:8]([C:22]3[CH:27]=[CH:26][C:25]([N+]([O-])=[O:29])=[CH:24][CH:23]=3)[C:7]=2[CH:31]=1.C(=O)(O)[O-].[Na+]>>[OH-:29].[NH:19]([C:13]1[N:12]2[C:6]3[CH:5]=[CH:4][C:3]([Cl:2])=[CH:31][C:7]=3[C:8]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[N:9][CH2:10][CH:11]2[N:15]([CH3:16])[NH+:14]=1)[C:20]1[CH:5]=[CH:4][CH:3]=[CH:31][CH:7]=1Participants
3
Procedure
The residue containing 1-anilino-8-chloro-3-methyl-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepinium chloride (VIII) (obtained in A, above) is mixed with cold, dilute aqueous sodium bicarbonate solution and extracted with chloroform. The extract is washed with brine, dried with sodium sulfate and concentrated. The residue is crystallized to give 1-anilino-8-chloro-3-methyl-6-phenyl-4H-s-triazolo-[4,3-a][1,4]benzodiazepinium hydroxide inner salt (XI).
Workup
- customobtained in A, above)
- extractionextracted with chloroform
- washThe extract is washed with brine
- dry with materialdried with sodium sulfate
- concentrationconcentrated
- customThe residue is crystallized
Sources & evidence
- ORD record
- ord-144f821416524a0caae2bbd541edbbcd
- Source dataset
- uspto-grants-1978_04
- Patent number
- US04082761
Reaction notes
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