HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 86735474, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Oxalic Acid | HCID 971 | — |
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | HCID 22758373 | HCID 22758373 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 86735474 | HCID 86735474 | — |
Reaction Steps
3.76 g of 2-(3,4-dimethoxyphenyl)-2-(2,3-epoxypropyl)-m-dithiane-1,1,3,3-tetraoxide are heated at reflux for 18 hours under argon with 50 ml of ethanol, 30 ml of chloroform and 1.95 g of N-methyl-homovetratrylamine. After evaporation of the solvent, the residue is chromatographed on silica gel with chloroform/ethanol (98:2). The oil obtained is dissolved in acetone and treated with an equivalent amount of anhydrous oxalic acid. The precipitate is filtered off and recrystallized from methanol/acetone. The racemic α- (3,4-dimethoxyphenethyl)-methylamino!-methyl-2-(3,4-dimethoxyphenyl)-m-dithiane-2-ethanol-1,1,3,3-tetraoxide oxalate (1:1) obtained crystallizes with 1 mol of acetone and melts at 162°-164° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04073797 |
| Source dataset | uspto-grants-1978_02 |
| ORD ID | ord-f9b1553e33ab4ac0a3f094d2e70fcabc |
| Source note | uspto-grants-1978_02 |