HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178428861, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 178428864 | HCID 178428864 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178428861 | HCID 178428861 | 75.9% |
Reaction Steps
1,1-dimethylethyl 3-({4-[({4-[(1H-benzimidazol-2-ylamino)carbonyl]-1H-imidazol-5-yl}carbonyl)amino]-3-methylphenyl}oxy)azetidine-1-carboxylate (155.0 mg, 0.29 mmol) was suspended in 5 mL of ethyl acetate, which was cooled with an ice-water bath. 3 mL of 4 N HCl in dioxane was added dropwise. The reaction mixture was stirred overnight. The suspension was filtered and the solid was washed with 5 mL of ethyl acetate, dried under vacuum to afford the desired product (102 mg, 0.22 mmol) as the hydrochloride salt. 1H-NMR (400 MHz, DMSO-d6): δ=10.9 (br, 1H), 9.85 (br, 2H), 8.32 (s, 1H), 7.63 (m, 2H), 7.38 (m, 3H), 6.84 (m, 1H), 6.78 (m, 1H), 5.05 (m, 1H), 4.43 (m, 2H), 3.94 (m, 2H), 2.25 (s, 3H). MS: 432 (M++1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08088767B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-7c216d5050df44eb9b099f0f43d26c85 |
| Source note | uspto-grants-2012_01 |