HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 6-(Azetidin-3-ylamino)-7-fluoro-4-methyl-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one hydrochloric acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 3-(7-Fluoro-4-methyl-3-oxo-2,3,4,10-tetrahydro-9-oxa-1,2,4a-triaza-phenanthren-6-ylamino)-azetidine-1-carboxylic acid tert-butyl ester | HCID 86727327 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 6-(Azetidin-3-ylamino)-7-fluoro-4-methyl-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one hydrochloric acid | HCID 86727328 | 31% |
Reaction Steps
To a suspension of 3-(7-fluoro-4-methyl-3-oxo-2,3,4,10-tetrahydro-9-oxa-1,2,4a-triaza-phenanthren-6-ylamino)-azetidine-1-carboxylic acid tert-butyl ester (0.110 g, 0.271 mmol) in EtOAc (10 mL) was added an EtOAc solution saturated with hydrogen chloride (3 mL). The reaction mixture was stirred at rt for 3 h then concentrated in vacuo and the residue was purified by preparative HPLC (Table 3, Method 1)) to give 6-(azetidin-3-ylamino)-7-fluoro-4-methyl-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one hydrochloric acid as a white solid (0.026 g, 31%). LC/MS (Table 1, Method 5) Rt=1.853 min.; MS m/z: 306 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115151B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-32d2c5b49090403ba8fe969ddca77bbf |
| Source note | uspto-grants-2015_08 |