Phosphorus oxychloride → HCID 22036901, compound
Reaction equation
O[C:2]1[C:3]2[S:10][C:9]([C:11]3[CH:16]=[C:15]([CH3:17])[CH:14]=[C:13]([CH3:18])[CH:12]=3)=[CH:8][C:4]=2[N:5]=[CH:6][N:7]=1.C(N(C(C)C)CC)(C)C.P(Cl)(Cl)([Cl:30])=O>>[Cl:30][C:2]1[C:3]2[S:10][C:9]([C:11]3[CH:16]=[C:15]([CH3:17])[CH:14]=[C:13]([CH3:18])[CH:12]=3)=[CH:8][C:4]=2[N:5]=[CH:6][N:7]=1Participants
4
Conditions
- Temperature
- 100 °C
Procedure
The hydroxy compound prepared in Step 1 was treated with phosphorous oxychloride (150 mL) and diisopropylethylamine (2 mL). The mixture was then heated at 100° C. for 4 hours. The solvents were evaporated under reduced pressure and the residue was carefully treated with ice water. The resulting solid was filtered off and crystallized from ethanol.
Workup
- customThe solvents were evaporated under reduced pressure
- additionthe residue was carefully treated with ice water
- filtrationThe resulting solid was filtered off
- customcrystallized from ethanol
Sources & evidence
- ORD record
- ord-b005b6f337a44f94b9a0bf0c978e4792
- Source dataset
- uspto-grants-2006_07
- Patent number
- US07071190B2
Reaction notes
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