Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | HCID 86713580 | HCID 86713580 | — |
| Product | HCID 86713579 | HCID 86713579 | 96% |
Reaction Steps
To a solution of 3-(3,5-dimethoxyphenyl)-1-methyl-7-(methylsulfonyl)-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one (400 mg, 1.06 mmol) in 15 mL of dichloromethane was added sulfuryl chloride (285 mg, 2.12 mmol) at 0° C., and then stirred at 0° C. for 3 h. LCMS showed the reaction was completed. The reaction mixture was diluted with 20 mL of dichloromethane, washed with water and brine, dried over sodium sulfate, filtered and concentrated to afford the title compound (450 mg, 96%) as a yellow solid, which was directly used in the next step without further purification. MS (ES+) C16H16Cl2N4O5S requires: 446, 448. Found: 447, 449 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09126951B2 |
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| Source dataset | uspto-grants-2015_09 |
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| ORD ID | ord-08c99551bffd4340be64ec36a7bb7b48 |
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| Source note | uspto-grants-2015_09 |
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