Phosphorus oxychloride → HCID 15391116, compound
Reaction equation
[CH2:1]([N:8]1[C:12]2=[N:13][CH:14]=[N:15][C:16](O)=[C:11]2[C:10]([C:18]2[O:19][CH:20]=[CH:21][CH:22]=2)=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1(C)C=CC=CC=1.C(OCC)(=O)C.O=P(Cl)(Cl)[Cl:38]>>[CH2:1]([N:8]1[C:12]2=[N:13][CH:14]=[N:15][C:16]([Cl:38])=[C:11]2[C:10]([C:18]2[O:19][CH:20]=[CH:21][CH:22]=2)=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1Participants
4
Procedure
6.6 g of 1-benzyl-3-(2-furyl)-4-hydroxypyrazolo[3,4-d]pyrimidine are boiled for 12 h in 100 ml of POCl3. The mixture is evaporated in vacuo, the residue is stirred with aqueous K2HPO4 solution and the mixture is extracted with ethyl acetate. After drying using Na2SO4 and concentrating in a rotary evaporator, 7.47 g of a solid are obtained which can be reacted directly for the next stage (Rf=0.8, SiO2, toluene/ethyl acetate=1:1).
Workup
- customThe mixture is evaporated in vacuo
- extractionthe mixture is extracted with ethyl acetate
- customAfter drying
- concentrationconcentrating in a rotary evaporator, 7.47 g of a solid
- customare obtained which
Sources & evidence
- ORD record
- ord-bc77d7ce9e4642af8d3f67eb05063ab7
- Source dataset
- uspto-grants-2002_09
- Patent number
- US06451805B1
Reaction notes
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