HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 71008464, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | HCID 71008528 | HCID 71008528 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 71008464 | HCID 71008464 | 66.7% |
Reaction Steps
In a sealed tube a solution of (R)-1-[1-(3-bromo-phenyl)-1H-pyrazol-4-yl]-3-cyanato-2,2-difluoro-1-methylpropylamine (3.0 g, 8.08 mmol) and ammonium hydroxide (25% in water, 7 ml) in methanol (10 ml) was heated to 60° C. for 16 hours. For the workup, the solution was evaporated at reduced pressure. The crude material thus obtained was purified by column chromatography on silica gel using a 95:5-mixture of dichloromethane and methanol as the eluent to give the (R)-4-[1-(3-bromo-phenyl)-1H-pyrazol-4-yl]-5,5-difluoro-4-methyl-5,6-dihydro-4H-[1,3]oxazin-2-ylamine (2.0 g, 54% yield) as a white solid. MS (ISP): m/z=371.2 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08785436B2 |
| Source dataset | uspto-grants-2014_07 |
| ORD ID | ord-d3a1b7a9ffb04282b2e523beb2dac9f4 |
| Source note | uspto-grants-2014_07 |