HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 20028646, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 4,4-Diethoxybutanenitrile | HCID 87616 | — |
| Reactant | HCID 14180973 | HCID 14180973 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Dichloromethane ethanol | HCID 21584144 | — |
| Product | HCID 20028646 | HCID 20028646 | 5.8% |
Reaction Steps
The compound of Example 29 Section (c) (1.5 g) was suspended in aqueous 25% acetic acid (10 ml) and 3-cyanopropanal diethyl acetal (0.237 g) was added. The mixture was heated at 80° for 2.5 h. The cooled reaction mixture was poured into NaOH solution (2N, 15 ml) and EA (15 ml) cooled in an ice-bath. K2CO3 (2 g) was added portionwise and the layers were separated. The aqueous layer was washed with EA (25 ml) and the combined organic extracts were dried (MgSO4) and evaporated in vacuo to give a yellow oil. The oil was dissolved in CH2Cl2 /ethanol/aqueous NH3 (200:8:1) and flash chromatographed using the same solvent system to give the title compound (33 mg) as a white solid, m.p. 187.5°-189°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04855314 |
| Source dataset | uspto-grants-1989_08 |
| ORD ID | ord-de26c7ba32f34cb4a232dc73edd9b95f |
| Source note | uspto-grants-1989_08 |