HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86708921, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 86708920 | HCID 86708920 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86708921 | HCID 86708921 | — |
Reaction Steps
To ethyl 2-(6,6-dioxido-7-(2,4,6-trichlorophenyl)-6-thia-5,7-diazaspiro[2,5]-octane-5-yl)acetate (60 mg, 0.14 mmol) in THF (5 mL) and MeOH (5 mL), was added LiOH monohydrate (25 mg, 0.58 mmol) in water (1 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 (50 mg, 89%, white solid). 1H NMR (300 MHz, CDCl3): δ 7.39 (s, 2H), 4.39 (s, 2H), 3.73 (s, 2H), 3.57 (s, 2H), 0.66-0.64 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09073906B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-6d2806e3aa7e4d9fbd0d9aac03d26591 |
| Source note | uspto-grants-2015_07 |