HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → Ethyl 2-(2-aminothiazol-4-yl)-2-methoxyiminoacetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | Thiourea | HCID 2723790 | — |
| Reactant | Ethyl 4-chloro-2-(methoxyimino)-3-oxobutanoate | HCID 3017525 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | Ethyl 2-(2-aminothiazol-4-yl)-2-methoxyiminoacetate | HCID 581091 | 68.5% |
Reaction Steps
Ethyl 2-methoxyimino-4-chloroacetoacetate (syn isomer) (50 g.) was added over 3 minutes with stirring at ambient temperature to a solution of thiourea (18.4 g.) and sodium acetate (19.8 g.) in a mixture of methanol (250 ml.) and water (250 ml.). After stirring for 35 minutes at 40° to 45° C., the reaction mixture was cooled with ice and adjusted to pH 6.3 with a saturated aqueous solution of sodium bicarbonate. After stirring for 30 minutes at the same temperature, precipitates were collected by filtration, washed with water (200 ml.) and then with diisopropyl ether (100 ml.), and dried to give colorless crystals of ethyl 2-methoxyimino-2-(2-amino-1,3-thiazol-4-yl)acetate (syn isomer) (37.8 g.), m.p. 161° to 162° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04604456 |
| Source dataset | uspto-grants-1986_08 |
| ORD ID | ord-3d85c218d8ac49c0ab39d0006b1d80ad |
| Source note | uspto-grants-1986_08 |