Phosphorus oxychloride → HCID 58192232, compound
Reaction equation
[C:1]1([C:7]2[N:12]=[C:11]3[C:13]4[CH:19]=[CH:18][CH:17]=[CH:16][C:14]=4[O:15][C:10]3=[C:9](O)[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O=P(Cl)(Cl)[Cl:23]>>[Cl:23][C:9]1[CH:8]=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[N:12]=[C:11]2[C:13]3[CH:19]=[CH:18][CH:17]=[CH:16][C:14]=3[O:15][C:10]=12Participants
3
Conditions
- Temperature
- 110 °C
Procedure
1D (53.6 mmol) was added to POCl3 (90 mL), heated to dissolve and stirred at 110° C. for 2.5 hours. TLC showed the reaction completed. POCl3 was evaporated under reduced pressure. The residue was cooled and poured into ice-water under stirring. The solids were collected by filtration and dried to give the desired product M1 (11.5 g).
Workup
- temperatureheated
- dissolutionto dissolve
- customPOCl3 was evaporated under reduced pressure
- temperatureThe residue was cooled
- additionpoured into ice-water
- stirringunder stirring
- filtrationThe solids were collected by filtration
- customdried
Sources & evidence
- ORD record
- ord-f6e8b3b3e5544fb6b385d522b14789c2
- Source dataset
- uspto-grants-2015_03
- Patent number
- US08969373B2
Reaction notes
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