Ammonia → HCID 178439841, compound
Reaction equation
[CH2:1]([C:4]1[NH:5][C:6]2[CH:12]=[C:11]3[NH:13][C:14](=[O:22])[C:15](C(OCC)=O)([CH3:16])[C:10]3=[CH:9][C:7]=2[N:8]=1)[CH2:2][CH3:3].S(=O)(=O)(O)O.N>>[CH2:1]([C:4]1[NH:5][C:6]2[CH:12]=[C:11]3[NH:13][C:14](=[O:22])[CH:15]([CH3:16])[C:10]3=[CH:9][C:7]=2[N:8]=1)[CH2:2][CH3:3]Participants
4
Procedure
1.50 g. (4.9 mmole) of the compound prepared in Example 10 is stirred in 30 ml. 60% sulphuric acid for 1 hour at 60° C. bath temperature, then poured on to ice, neutralised with 2N aqueous ammonia solution and the precipitated product is filtered off with suction and the residue crystallised from ethyl acetate/methanol. There is obtained 0.70 g. (62% of theory) of the title compound; m.p. 235°-238° C.
Workup
- additionpoured on to ice
- filtrationthe precipitated product is filtered off with suction
- customthe residue crystallised from ethyl acetate/methanol
- customThere is obtained 0.70 g
Sources & evidence
- ORD record
- ord-8f4172160fe34fab90456ce516185ef4
- Source dataset
- uspto-grants-1988_03
- Patent number
- US04730003
Reaction notes
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