HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 86649114, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | tert-Butanol | HCID 6386 | — |
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | 2-Bromo-4'-nitroacetophenone | HCID 66840 | — |
| Reactant | 4'-Chloro-3'-nitroacetophenone | HCID 79596 | — |
| Catalyst | Zincchloride | HCID 3007855 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 86649114 | HCID 86649114 | — |
Reaction Steps
To a mixture of zinc chloride (39.1 g, 287 mmol) in benzene (215 mL) was added diethylamine (22.24 mL, 215 mmol) and 2-methylpropan-2-ol (20.57 mL, 215 mmol). The resulting mixture was stirred at rt for 2 h, and 2-bromo-1-(4-nitrophenyl)ethanone (35.0 g, 143 mmol) and 1-(4-chloro-3-nitrophenyl)ethanone (42.9 g, 215 mmol) were added in one portion. The resulting mixture was stirred at rt overnight. Added 5% aq. H2SO4 (50 mL) and stirred vigorously to induce precipitation. The resulting solid was collected by filtration and washed successively with benzene, water, methanol, and CH2Cl2. The solid was dried in vacuo to give the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09006387B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-9e20942ad50d4a1aa8100678a2afa2c9 |
| Source note | uspto-grants-2015_04 |