HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 68412077, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | tert-Butyldimethylsilyl trifluoromethanesulphonate | HCID 123564 | — |
| Reactant | HCID 13981853 | HCID 13981853 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 68412077 | HCID 68412077 | — |
Reaction Steps
2,6-Lutidine (3.6g) was added to an anhydrous methylene chloride solution of benzyl 3-hydroxy-3-methylbutyrate (3.5g) obtained in the step 1, and stirred with cooling with ice. t-butyldimethylsilyl trifluoromethanesulfonate (3.9mL) was gradually added dropwise thereto, and stirred for 1hour with cooling on ice and then for 2hours at room temperature. The reaction liquid was diluted with ethyl acetate, then washed with water, aqueous saturated ammonium chloride solution and aqueous saturated sodium chloride solution, then dried over anhydrous magnesium sulfate and concentrated. 4.5g of the residue was purified through silica gel column chromatography to give benzyl 3-(t-butyldimethylsilyloxy)-3-methylbutyrate (2.62g) as a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796246B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-d95339e0cec5445bb7d4ea97ec0a8d21 |
| Source note | uspto-grants-2014_08 |