HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 10228153, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3,3-Dimethylbutanoyl chloride | HCID 81514 | — |
| Reactant | HCID 11361321 | HCID 11361321 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10228153 | HCID 10228153 | — |
Reaction Steps
59 mg (0.150 mmol) of the compound from Example XIV and 0.04 ml (0.30 mmol) of triethylamine are initially-charged in 5 ml of dichloromethane. At 0° C., a solution of 26 mg of 3,3-dimethylbutyryl chloride (0.195 mmol) in 1 ml of dichloromethane is added dropwise, and the mixture is stirred at RT for 30 min. The reaction solution is concentrated and the residue is purified chromatographically on silica gel 60 (mobile phase gradient cyclohexane→cyclohexane:ethyl acetate 2.5:1). The resulting product is taken up in a little ethyl acetate, precipitated by addition of n-pentane, filtered off with suction and dried. This gives 35 mg (45% of theory) of a light-beige solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07045544B2 |
| Source dataset | uspto-grants-2006_05 |
| ORD ID | ord-a0dd689787f7498fa7b1696c69ed5781 |
| Source note | uspto-grants-2006_05 |