HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Chlorobenzoic Acid → 3-Chlorobenzoyl 1-methyl-1-propyl carbonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Chlorobenzoic Acid | HCID 447 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | sec-Butyl chloroformate | HCID 11829505 | — |
| Solvent | Water | HCID 962 | — |
| Product | 3-Chlorobenzoyl 1-methyl-1-propyl carbonate | HCID 86591390 | 97.4% |
Reaction Steps
To a well-stirred reaction vessel equipped with a thermometer and a pH electrode were added 39 g of water and 0.20 g of Arquad CB50 at 5° C. After the addition of 0.05 mole of 3-chlorobenzoic acid the pH was adjusted to 6 using a 10 wt % aqueous NaOH solution. Then, 0.05 mole of sec-butyl chloroformate was dosed within 5 min at 5° C. During this time and a post-reaction time of 165 min at 5° C. the pH was kept at a value between 6 and 9. The reaction mixture was allowed to separate, giving 12.5 g of 3-chlorobenzoyl 1-methyl-1-propyl carbonate having a content of 98% in a yield of 95%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06610880B1 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-08e8848c0b2c4f53a157200aa871f770 |
| Source note | uspto-grants-2003_08 |