HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 68295008, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 86700716 | HCID 86700716 | — |
| Product | HCID 68295008 | HCID 68295008 | 79% |
Reaction Steps
To a mixture of conc. H2SO4 (2.5 ml) and methanol (7.5 ml) was added [4-(3,4-Difluoro-phenyl)-2-methyl-1-oxo-1,2-dihydro-isoquinolin-3-y]-trimethylsilanyloxy-acetonitrile (580 mg, 1.45 mmol), after addition, the resultant mixture was stirred at reflux overnight under N2. TLC showed SM was consumed, diluted with EA, adjusted with saturated NaHCO3 to pH=8˜9, extracted with EA, the organic layers was dried over Na2SO4 and concentrated to dryness to afford crude product. (m=430 mg, yield=79%). LCMS: (10-80 AB—2MIN-E.M): Rt=1.021, purity=64%, M+1=360.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029391B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-791a02559f55455691b86239c2376716 |
| Source note | uspto-grants-2015_05 |