HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzoyl chloride → HCID 13032033, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzoyl chloride | HCID 7412 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | O-(Tetrahydropyran-2-yl)hydroxylamine | HCID 5142091 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 13032033 | HCID 13032033 | 77% |
Reaction Steps
To a solution of 1.00 g (8.55 mmol) of O-tetrahydropyran-2-ylhydroxylamine (prepared as described in U.S. Pat. No. 4,607,053, Example 2, Part A) and 1.4 ml (10 mmol) of sieve-dried triethylamine in 15 ml of dry CH2Cl2 cooled to -20 was added a solution of 1.50 g (10.7 mmol) of benzoyl chloride in 5 ml of CH2Cl2 over 10 minutes. The reaction mixture was stirred for 1 hour then diluted with 15 ml of ethyl acetate. The resulting slurry was filtered and the filtrate concentrated in vacuo to give a solid. Recrystallization (EtOAc/petroleum ether) of the solid afforded 1.45 g (77%) of title compound as white crystals, m.p. 130°-134°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04757078 |
| Source dataset | uspto-grants-1988_07 |
| ORD ID | ord-a7c4e1d1a15c4fe1a9f89e0c0e26d8ea |
| Source note | uspto-grants-1988_07 |