HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 89599450, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,2,2-Trichloroethyl 3-tert-butyl-1-P-tolyl-1H-pyrazol-5-ylcarbamate | HCID 9931094 | — |
| Reactant | HCID 89599243 | HCID 89599243 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 89599450 | HCID 89599450 | 45% |
Reaction Steps
A solution of Example 20 step b (60 mg, 0.11 mmol), DIPEA (26 μL, 0.15 mmol) and 2,2,2-trichloroethyl 3-tert-butyl-1-p-tolyl-1H-pyrazol-5-ylcarbamate (56 mg, 0.138 mmol) in dioxane (5 mL) was heated at 80° C. for 20 h. The reaction was allowed to cool to RT, partitioned between H2O-DCM, the organic phase dried (MgSO4) and concentrated in vacuo. The residue was purified by FCC using MeOH in DCM (0 to 5%) to give the title compound as a yellow foam (38 mg, 45%). LCMS (Method 3): Rt 4.09 min, m/z 772 [MH+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916708B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-d114053f94aa47368a15e88ef6fed62a |
| Source note | uspto-grants-2014_12 |