Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1-(3H-Imidazo[4,5-c]pyridin-2-yl)methanamine | HCID 33726567 | — |
| Reactant | 4-Chloro-2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidine 5-oxide | HCID 59475895 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 59708428 | HCID 59708428 | 19.4% |
Reaction Steps
200 mg 4-chloro-2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidine 5-oxide (cf Example 124), 346.22 mg C-(3H-imidazo[4,5-c]pyridin-2-yl)-methylamine and 359.24 μl diisopropylethylamine are placed in 4 ml dioxane, heated to 120° C. in the microwave for 0.3 hours and heated for another 0.3 hours at 120° C. Then the reaction mixture is mixed with water. The precipitated substance is suction filtered and washed with water. The product is purified by semipreparative HPLC (method A). 50 mg of the product are obtained as a powder. Analytical HPLC-MS (method B): RT=1.55 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08604039B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-2b0f243f758349bd81a9590764ff6fd9 |
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| Source note | uspto-grants-2013_12 |
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