HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86708919, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 86708917 | HCID 86708917 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86708919 | HCID 86708919 | — |
Reaction Steps
To ethyl 2-(4-methylene-1,1-dioxido-6-(2,4,6-trichlorophenyl)-1,2,6-thiadiazinan-2-yl)acetate (305 mg, 0.74 mmol) in THF (10 mL) and MeOH (10 mL), was added LiOH monohydrate (155 mg, 3.69 mmol) in water (3 mL) and agitated for 5 hr at room temperature. After addition of ethyl acetate (30 mL) and water (30 mL), pH of the resultant was adjusted to 3 with 1 N HCl and extracted to the organic layer. The resultant was dried over MgSO4, concentrated under reduced pressure, and crystallized with ethyl acetate (1 mL) and hexane (10 mL), giving the compound of interest (253 mg, 89%, white solid). 1H NMR (300 MHz, CDCl3): δ 7.42 (s, 2H), 5.26 (s, 1H), 5.16 (s, 1H), 4.41 (s, 2H), 4.33 (s, 2H), 4.09 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09073906B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-0a20bf8b96ef463e88a45783c84f668e |
| Source note | uspto-grants-2015_07 |