Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 12093240 | HCID 12093240 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 12093239 | HCID 12093239 | — |
Reaction Steps
3.5 ml isopropanolic hydrochloric acid (5-6 M) are added to 340 mg of 1-[(1-methyl-2,2-dioxo-1H-benzo[c][1,2]thiazin-4-yl)methyl]-3-methyl-7-(3-methyl-2-buten-1-yl)-8-[3-(tert.-butyloxycarbonylamino)-piperidin-1-yl]-xanthine in 15 ml methylene chloride and the reaction mixture is stirred for three hours at ambient temperature. For working up it is diluted with water and methylene chloride and combined with 18 ml 1N sodium hydroxide solution. The aqueous phase is extracted with methylene chloride and the combined organic phases are washed with water, dried over magnesium sulphate and evaporated down. The yellowish, foamy flask residue is stirred with tert.-butyl-methylether and a little diethyl ether, the light-coloured precipitate formed is suction filtered and dried at 60° C. in the drying gun.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07482337B2 |
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| Source dataset | uspto-grants-2009_01 |
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| ORD ID | ord-e2d8a311e7884116874978afaf4e3b04 |
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| Source note | uspto-grants-2009_01 |
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