HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,5-Di-tert-butyl-4-hydroxybenzaldehyde → 2-Amino-5-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-4(5H)-thiazolone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,5-Di-tert-butyl-4-hydroxybenzaldehyde | HCID 73219 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | (5Z)-5-[(3-cyclopentyloxy-4-methoxyphenyl)methylidene]-2-imino-1,3-thiazolidin-4-one | HCID 137629131 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 2-Amino-5-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-4(5H)-thiazolone | HCID 137244729 | 70.7% |
Reaction Steps
A mixture of 3,5-di-tert-butyl-4-hydroxybenzaldehyde (9.4 g, 0.04 mole), pseudothiohydantoin (4.7 g, 0.0405 mole), sodium acetate (8.3 g, 0.1 mole), and glacial acetic acid (200 mL) is stirred and heated at reflux for 21 hours. The cooled mixture is added to ice-water and the precipitated solid is filtered and washed with water. The solid residue is dissolved in ether and washed successively with water, aqueous sodium bicarbonate solution, and water. The extract is dried and the solvent is removed to give 9.4 g of a residue. The crude product is recrystallized from methanol-ethyl acetate to give 3.8 g (38%) of 5-[[3,5-Bis(1,1-dimethylethyl)-4-hydroxyphenyl]methylene]-2-imino-4-thiazolidinone, (Z)-, mp 277°-279° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05143928 |
| Source dataset | uspto-grants-1992_09 |
| ORD ID | ord-be5e41cab14c4cd1abecc15df068ea37 |
| Source note | uspto-grants-1992_09 |