HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → Ethyl 2-(3-bromo-5-chloro-4-hydroxyphenyl)acetate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | Ethyl 2-(3-bromo-4-hydroxyphenyl)acetate | HCID 18620106 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Ethyl 2-(3-bromo-5-chloro-4-hydroxyphenyl)acetate | HCID 57995583 | 60% |
Reaction Steps
To a stirred solution of ethyl 2-(3-bromo-4-hydroxyphenyl)acetate (20 g, 0.076 molo) in 200 ml of DCM was added MeOH (3.4 ml, 0.84 mol) and the mixture was refluxed. Sulfuryl chloride (6.8 ml 0.846 mol) was slowly added under over a period of 10 min. The reaction mixture was refluxed for a further 5 h. Upon completion of reaction, the mixture was poured onto crushed ice and extracted with DCM (×2). The combined organic layer were washed with 10% NaHCO3 solution and water, dried over Na2SO4, filtered and evaporated under vacuum to give ethyl 2-(3-bromo-5-chloro-4-hydroxyphenyl)acetate in 60% yield. (13.6 g). 1HNMR (CDCl3): 7.37 (s, 1H); 7.27 (s, 1H); 5.68 (bs, 1H); 4.16 (q, 2H); 3.48 (s, 2H); 1.29 (t, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367863B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-4beb0ad174d2457184490062355a32c1 |
| Source note | uspto-grants-2013_02 |