HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → ETHYL 2-METHYLBENZOYLFORMATE
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Diethyl Oxalate | HCID 7268 | — |
| Product | ETHYL 2-METHYLBENZOYLFORMATE | HCID 11622483 | 30.3% |
Reaction Steps
A solution of 83 g of diethyl oxalate in toluene (170 g) was cooled to −40° C. or lower. The Grignard reagent prepared as described above was added dropwise at −40° C. or lower, and this was retained at −40° C. for 2 hours. To the reaction mixture was added 234 g of 10% sulfuric acid, and an organic layer was recovered. The resulting organic layer was washed with 134 g of water, and dried with magnesium sulfate. After concentration with an evaporator, distillation under high vacuum, and silica gel column purification afforded 33.1 g of ethyl 2-(methyl-phenyl)-2-oxoacetate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08192967B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-e75571c12e1a4dc3a41808944d4ca378 |
| Source note | uspto-grants-2012_06 |