Phosphorus oxychloride → HCID 22763500, compound
Reaction equation
[Br:1][C:2]1[CH:19]=[CH:18][C:5]2[S:6][C:7]([C:15]([NH2:17])=O)=[C:8]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[C:4]=2[CH:3]=1.P(Cl)(Cl)(Cl)=O>>[Br:1][C:2]1[CH:19]=[CH:18][C:5]2[S:6][C:7]([C:15]#[N:17])=[C:8]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[C:4]=2[CH:3]=1Participants
3
Procedure
Reflux 2.1 g. 5-bromo-3-phenylbenzo [b ]thiophene-2-carboxamide (0.0063 mole) together with 10 ml. of phosphorus oxychloride for 11/2 hours and then carefully pour onto ice water. Filter off the white precipitate. Dry. Recrystallize the title compound from methanol; m.p. 145°-146°.
Workup
- temperatureReflux 2.1 g
- filtrationFilter off the white precipitate
- customDry
- customRecrystallize the title compound from methanol
Sources & evidence
- ORD record
- ord-b524d52c5d2e4b14aeb2b10c82cfeb87
- Source dataset
- uspto-grants-1976_12
- Patent number
- US03996159
Reaction notes
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