HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 131727051, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 1,2,3,3a,7,7a-Hexahydro-4-thia-2-aza-cyclopenta[alpha]pentalene | HCID 59789433 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 131727051 | HCID 131727051 | — |
Reaction Steps
Triethylamine (741 mg, 7.32 mmol) was added to a solution of the product from step h) (493 mg, 2.44 mmol) in 12 mL of CH2Cl2 at ° C. followed by the addition of ethyl chloroformate (529 mg, 4.88 mmol). The reaction was allowed to come to room temperature and was stirred for two hours. The reaction mixture was diluted with brine (15 mL) and extracted with dichloromethane (3×15 mL). The combined organic extracts were dried with MgSO4 and the solvent was evaporated in vacuo give the crude product that was purified by column chromatography (SiO2) using a 0-30% ethyl acetate-hexane gradient to give the subtitle compound. MS calculated for C12H15NO2S+H: 238, observed: 238.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07423056B2 |
| Source dataset | uspto-grants-2008_09 |
| ORD ID | ord-056ac90560d6431bbd9b50aa1d53ffb7 |
| Source note | uspto-grants-2008_09 |