HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → ethyl 3,3,3-trifluoro-2-hydroxypropanoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 3,3,3-Trifluoro-2-hydroxypropanoic acid | HCID 244896 | — |
| Product | ethyl 3,3,3-trifluoro-2-hydroxypropanoate | HCID 2758935 | 68% |
Reaction Steps
The step (b) of the present invention was conducted as follows. At first, 2.84 g of the crude product obtained by Example 1 (containing 16.07 mmol (1.00 eq.) of 3,3,3-trifluoro-2-hydroxypropionic acid) and 19.6 mg (0.20 mmol, 0.01 eq.) of 98% sulfuric acid were added to 20 ml of ethanol, followed by stirring for 43 hr with heating under reflux. The resulting reaction liquid itself was subjected to a vacuum distillation (52° C./3,500 Pa), thereby obtaining 1.87 g of white, needle-like crystals of ethyl 3,3,3-trifluoro-2-hydroxypropionate of the following formula 8. The yield was 68%. The obtained crude product (the white, needle-like crystals) was used in the following step (c) of Example 3 without conducting a further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06815559B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-1cf44ed070064de390d36da643351433 |
| Source note | uspto-grants-2004_11 |