HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 54718074, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | 3-Amino-5-methylisoxazole | HCID 66172 | — |
| Reactant | HCID 21530394 | HCID 21530394 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 54718074 | HCID 54718074 | 53.8% |
Reaction Steps
A mixture of 17 g (0.05 mol) of crude methyl 2,3,4,5-tetrahydro-5-oxo-1-benzothiepin-4-carboxylate 1,1-dioxide, 6.0 g (0.061 mol) of 3-amino-5-methylisoxazole, and 350 ml of toluene was refluxed for 24 hours in a Soxhlet apparatus the thimble of which contained 20 g of Linde type 4A molecular sieve. The mixture was diluted with 500 ml of ether and the resulting precipitate (10 g) was collected and recrystallized from 400 ml of tetrahydrofuran to give 9.0 g of product mp 226°-228°. Recrystallization gave an analytical sample mp 227°-229°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03962261 |
| Source dataset | uspto-grants-1976_06 |
| ORD ID | ord-dcd091349d814d71a5c472119a0d7f9a |
| Source note | uspto-grants-1976_06 |