HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isovaleryl chloride → HCID 57675214, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isovaleryl chloride | HCID 66054 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 67529443 | HCID 67529443 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 57675214 | HCID 57675214 | — |
Reaction Steps
Isovaleryl chloride (0.04 mmol) was added to a stirred solution of Intermediate 125 (0.033 mmol) and diisopropylethylamine (0.1 mmol) in chloroform (1 ml) at room temperature. After stirring at room temperature for 1.5 h, the reaction mixture was applied to a SPE cartridge (aminopropyl, 1 g) and the cartridge was eluted sequentially with chloroform, ethyl acetate and methanol. Fractions containing the desired product were combined and blown down under nitrogen. The resulting residue was further purified on a SPE cartridge (silica, 1 g) eluting with a gradient of 30-100% ethyl acetate in petroleum ether to afford Example 176. LCMS showed MH+=496, TRET=3.17 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07528148B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-f03eda8da05b43dd84fd8d0945ad6999 |
| Source note | uspto-grants-2009_05 |