Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 21183760 | HCID 21183760 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21183724 | HCID 21183724 | 49.8% |
Reaction Steps
50 ml of pyridine are added to a suspension of 9.5 g (29.7 mmol) of 1-(hydroxymethyl)-5,8-dimethyl-3-phenyl-3,5-dihydro-4H-pyridazino[4,5-b]indol-4-one in 600 ml of tetrahydrofuran heated to 60° C. 4.5 ml (59.4 mmol) of methanesulphonyl chloride are added and the mixture is left standing for 15 h at room temperature. 500 ml of dichloromethane are added, the precipitate is removed by filtration, separation is carried out by settling and the organic phase is washed with water. It is dried over sodium sulphate and the solvent is evaporated under reduced pressure. 5 g (14.8 mmol) of product are obtained, which product is used as is in the following stage.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06262045B1 |
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| Source dataset | uspto-grants-2001_07 |
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| ORD ID | ord-89e93adc666b45deac5d833f86be0e1b |
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| Source note | uspto-grants-2001_07 |
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