Methyl chloroformate → HCID 14474060, compound
Reaction equation
[OH:1][CH:2]1[O:7][CH2:6][C:5](=[O:8])[CH:4]=[CH:3]1.[C:9](Cl)(=[O:12])[O:10][CH3:11].C(N(CC)CC)C>C(Cl)Cl>[CH3:11][O:10][C:9]([O:1][CH:2]1[O:7][CH2:6][C:5](=[O:8])[CH:4]=[CH:3]1)=[O:12]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
12 g of 6-hydroxy-2H-pyran-3(6H)-one was dissolved in 100 ml of methylene chloride, and the solution was cooled to 0° C. Then, 9.4 g of methyl chlorocarbonate was added thereto, and a solution comprising 10.6 g of triethylamine and 20 ml of methylene chloride was dropwise added thereto. The mixture was stirred for 3 hours, and the reaction mixture was poured into ice water and extracted with methylene chloride. The solvent was distilled off under reduced pressure, and the residue was subjected to distillation under reduced pressure to obtain 10.3 g (yield: 60%) of the above-identified compound.
Workup
- additionwas dropwise added
- extractionextracted with methylene chloride
- distillationThe solvent was distilled off under reduced pressure
- distillationthe residue was subjected to distillation under reduced pressure
Sources & evidence
- ORD record
- ord-4f16f0ebb7da42138c87ee66329074d0
- Source dataset
- uspto-grants-1989_06
- Patent number
- US04837345
Reaction notes
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