HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,3-Dichlorobenzaldehyde → HCID 19980840, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,3-Dichlorobenzaldehyde | HCID 35745 | — |
| Reactant | tert-Butyl 6-oxo-1,4-thiazepane-4-carboxylate 1,1-dioxide | HCID 19980844 | — |
| Reactant | HCID 19980851 | HCID 19980851 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 19980840 | HCID 19980840 | 34.6% |
Reaction Steps
A mixture of 4-N-(t-butyloxycarbonyl)-1,1-dioxo -2,3,4,5,6,7-hexahydro-1,4-thiazepine-6-one (9.06 g, 34.5 mmole) from Example 6, 2,3-dichlorobenzaldehyde (6.03 g, 34.5 mmole) and 2-hydroxyethyl 3-aminocrotonate (5.00 g, 34.5 mmole) was heated to reflux in 200 mL of ethanol for 24 hours. The ethanol was removed under reduced pressure and the residue was heated in refluxing toluene for 2 hours. After cooling a precipitate was filtered to give 6.75 g of the title compound. Evaporation of the filtrate and chromatography (2.5:1, ethyl acetate:hexane) produced 3.78 g of product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05075440 |
| Source dataset | uspto-grants-1991_12 |
| ORD ID | ord-466761ee21084fa98a049d377c505574 |
| Source note | uspto-grants-1991_12 |