HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 20552955, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Aminobenzophenone | HCID 76080 | — |
| Reactant | Tert-Butyl hypochlorite | HCID 521297 | — |
| Reactant | Acetamide, N,N-dimethyl-2-(methylthio)- | HCID 11815402 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 20552955 | HCID 20552955 | 81% |
Reaction Steps
A solution of 29.6 g (0.15 mole) of 2-aminobenzophenone in 350 ml of methylene chloride was cooled to -70° C. and 20.0 g (0.15 mole) of 2-methylthio-N,N-dimethylacetamide was added. To the mixture (-70° C.) was added dropwise a solution of 17.2 g (0.15 mole) of 95% t-butylhypochlorite in 30 ml of methylene chloride. The temperature was maintained at or below -65° C. for 1.5 hr, then 15.1 g (0.15 mole) of triethylamine was added rapidly. The solution was allowed to warm to room temperature and was washed with water. The organic solution was concentrated and the residue crystallized when mixed with isopropyl ether. The solid was recrystallized from isoproyl alcohol to give 39.8 g (81%) bright yellow crystals, m.p. 153°-155° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04313949 |
| Source dataset | uspto-grants-1982_02 |
| ORD ID | ord-8e2f04d40c0a4102b0df095170dfc4b3 |
| Source note | uspto-grants-1982_02 |