HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,3-Dimethylbutanoyl chloride → HCID 59253284, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,3-Dimethylbutanoyl chloride | HCID 81514 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 43115327 | HCID 43115327 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59253284 | HCID 59253284 | 70.4% |
Reaction Steps
To a solution of 4-bromo-N1-(cyclopropylmethyl)benzene-1,2-diamine (Step B, 11.3 g, 46.9 mmol) and N,N-diisopropylethylamine (6.06 g, 46.9 mmol) in ethyl acetate (88 mL) was added tert-butylacetyl chloride (6.31 g, 46.9 mmol) at 0° C. and the mixture was allowed to warm to room temperature for 15 h. The reaction mixture was washed with saturated sodium hydrogen carbonate aqueous solution (100 mL×2), brine (50 mL). The resulting ethyl acetate solution of reaction mixture was dried over magnesium sulfate and concentrated under reduced pressure. The crude product was washed with ethyl acetate to afford the title compound (11.2 g, 70%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07700618B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-7f08a077e4354aecb32b9b6225f77b84 |
| Source note | uspto-grants-2010_04 |