HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 59402311, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Methyl [2-(4-bromophenyl)-1-methylethyl]carbamate | HCID 59402313 | — |
| Product | HCID 59402311 | HCID 59402311 | 100.8% |
Reaction Steps
To a mixture of methyl [2-(4-bromophenyl)-1-methylethyl]carbamate (465 mg, 1.71 mmol) and paraformaldehyde (82.1 mg, 2.73 mmol) was added a mixture of concentrated sulfuric acid (2.5 mL, 47 mmol) and glacial acetic acid (3.75 mL, 66.0 mmol). The resulting mixture was stirred at r.t. overnight. The reaction mixture was poured into ice-water, and extracted with CH2Cl2. The organic layer was washed with water, saturated NaCO3 aqueous solution and brine, dried with MgSO4. After filtration, the filtrate was concentrated to afford the desired compound (490 mg, 100%) which was directly used in the next step reaction without further purification. LCMS (M+H)+: m/z=284.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08436008B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-43e07e5a7212440e853a12d16a3de3f5 |
| Source note | uspto-grants-2013_05 |