Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 5,7-Dichloro-6-methylpyrazolo[1,5-a]pyrimidine | HCID 12366073 | — |
| Product | HCID 57752942 | HCID 57752942 | — |
Reaction Steps
A suspension prepared by adding POCl3 (3 mL) to N,N-dimethylformamide (9 mL) under nitrogen flow at room temperature was stirred for 5 min. To the suspension was slowly added 5,7-dichloro-6-methylpyrazolo[1,5-a]pyrimidine (5 g) and the reaction was carried out by heating the resulting viscous mixture solution at 70° C. for 3 hrs. The reaction mixture was poured into ice and the resultant solution was made alkaline with sodium hydroxide (5 g). The precipitate was filtered off and the dried precipitate was purified by silica gel chromatography (eluting with CH2Cl2→20% ethyl acetate/CH2Cl2) to obtain the title compound (3.74 g); the melting point was between 137 and 139° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07667036B2 |
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| Source dataset | uspto-grants-2010_02 |
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| ORD ID | ord-e715dd89c9b043088e83719fef50dcb9 |
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| Source note | uspto-grants-2010_02 |
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