Water → HCID 19787778, compound
Reaction equation
[C:1]1([C:7]2[N:12]=[C:11]([CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:10](=O)[NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.P(Cl)(Cl)([Cl:24])=O>>[Cl:24][C:10]1[N:9]=[N:8][C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)=[N:12][C:11]=1[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1Participants
4
Procedure
Heat a solution of 15 mmol (4 g) of 3-phenyl-5-benzyl-1,2,4-triazin-6-one obtained in Step C of Example 28 in 30 ml of phosphorus oxychloride to a temperature of 80° C. After cooling, pour into iced water, render alkaline and extract with ethyl acetate. Dry the organic phase, filter, evaporate to dryness and purify by chromatography on silica (eluant ethyl acetate/hexane: 27/75)
Workup
- temperatureAfter cooling
- extractionextract with ethyl acetate
- customDry the organic phase
- filtrationfilter
- customevaporate to dryness
- custompurify by chromatography on silica (eluant ethyl acetate/hexane: 27/75)
Sources & evidence
- ORD record
- ord-eedb14be5ffc41c09fa0ec12526ae4ac
- Source dataset
- uspto-grants-1993_10
- Patent number
- US05254548
Reaction notes
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