HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 68712508, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 68710411 | HCID 68710411 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 68712508 | HCID 68712508 | — |
Reaction Steps
To (3,5-Dimethyl-4-nitro-phenyl)-(4-trifluoromethyl-benzyl)-carbamic acid tert-butyl ester (9.5 g) in ethanol (150 mL) was added zinc dust (22 g) and acetic acid (13 mL). The reaction mixture was stirred 3 hours and then filtered. The solution was concentrated in vacuo, redissolved in ethyl acetate (100 mL) and extracted with water (2×50 mL). The organic phase was dried (MgSO4), filtered and concentrated in vacuo to give the title compound as an off white compound. Yield. 6.5 g (78%). LC-MS (m/z) 395 (MH+); tR=3.06, (UV, ELSD) 89%, 96%. 1H NMR (500 MHz, CDCl3): 1.40 (s, 9H), 2.10 (s, 6H), 3.50 (broad, 2H), 4.75 (s, 2H), 6.70 (s, 2H), 7.35 (d, 2H), 7.55 (d, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07601870B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-2289eeedc5114e9aacde00dc2ac74e22 |
| Source note | uspto-grants-2009_10 |