HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 2-[2,3-Dichloro-4-(2-methylenebutyryl)phenoxy]-2-methylpropionic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Dimethylamine, hydrochloride | HCID 10473 | — |
| Reactant | 2-(2,3-Dichloro-4-butyrylphenoxy)-2-methylpropionic acid | HCID 20148702 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-[2,3-Dichloro-4-(2-methylenebutyryl)phenoxy]-2-methylpropionic acid | HCID 14099860 | 61.4% |
Reaction Steps
A mixture of 2-(2,3-dichloro-4-butyrylphenoxy)-2-methylpropionic acid (10 g, 0.031 mole), dimethylamine hydrochloride (15 g, 0.18 mole), paraformaldehyde (3 g, 0.10 equiv.) and acetic acid (0.6 ml) was stirred and heated on a steam bath for two hours. N,N-dimethylformamide (30 ml) was added and stirring and heating was continued for another two hours. The mixture was poured into ice water which was then extracted with ether. The ether extract was washed with water, then brine and finally dried over MgSO4. The ether was evaporated in vacuo and the residue recrystallized from cyclohexane to give 6.3 g 2-[2,3-dichloro-4-(2-methylenebutyryl)phenoxy]-2-methylpropionic acid, m.p. 88°-89° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04731473 |
| Source dataset | uspto-grants-1988_03 |
| ORD ID | ord-4a0cf2d169dd474498ba0795c310d8e7 |
| Source note | uspto-grants-1988_03 |