HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Propene, 1,1-diethoxy- → cis-N-(4'-chlorobenzyl)-2,2-diethoxy-3,6-dimethyl-4-ethoxy-3,4-dihydro-2H-pyran-5-carboxamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Propene, 1,1-diethoxy- | HCID 140841 | — |
| Reactant | N-(4'-chlorobenzyl)-2-ethoxymethylene-3-oxobutanamide | HCID 53883739 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | cis-N-(4'-chlorobenzyl)-2,2-diethoxy-3,6-dimethyl-4-ethoxy-3,4-dihydro-2H-pyran-5-carboxamide | HCID 86746201 | 44% |
Reaction Steps
N-(4'-chlorobenzyl)-2-ethoxymethylene-3-oxobutanamide (1.4 g) and tris (6,6,7,7,8,8,8-heptafluoro-2,2-dimethyl-3,5-octanedianato)ytterbium (0.26 g) were stirred in toluene (10 ml) whilst 1,1-diethoxyprop-1-ene (4 g) was added dropwise. The mixture was stirred at room temperature for 3 days and evaporated to dryness. The residual gum was triturated with petroleum ether b.p. 60°-80° C. to give a solid which was recrystallised from a mixture of toluene and petroleum ether b.p. 60°-80° C. to give cis-N-(4'-chlorobenzyl)-2,2-diethoxy-3,6-dimethyl-4-ethoxy-3,4-dihydro-2H-pyran-5-carboxamide (0.9 g) m.p. 97°-100° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05296613 |
| Source dataset | uspto-grants-1994_03 |
| ORD ID | ord-6f0459269a0243bdb9d1cacd2f2da108 |
| Source note | uspto-grants-1994_03 |