Carbonochloridic acid (2,2-dimethyl-1,3-dioxolan-4-yl)methyl ester synthesis
- Product Name:Carbonochloridic acid (2,2-dimethyl-1,3-dioxolan-4-yl)methyl ester
- CAS Number:28863-62-9
- Molecular formula:C7H11ClO4
- Molecular Weight:194.61
Yield:28863-62-9 20%
Reaction Conditions:
Stage #1: bis(trichloromethyl) carbonatewith sodium carbonate;N,N-dimethyl-formamide in toluene; for 0.5 h;Cooling with ice;
Stage #2: (R,S)-2,2-dimethyl-1,3-dioxolane-4-methanol in toluene at 20; for 5 h;
Steps:
1
4.47 g (15.1 mmol) of triphosgene was taken in a recovery flask, and 60 ml of toluene was added to dissolve. Under ice-cooling, 3.22 g (30.4 mmol) of sodium carbonate and 70 μl (0.91 mmol) of N, N-dimethylformamide were added and the mixture was stirred for 30 minutes,2,2-dimethyl-1,3-dioxolane-4-methanolA solution of 4.14 g (31.3 mmol) of toluene in 60 ml was added dropwise. After stirring at room temperature for 5 hours, sodium carbonate was filtered off and the filtrate was concentrated under reduced pressure. The obtained residue was distilled under reduced pressure (1.0 kPa, distillation temperature: 70 to 83 ° C.) to obtain 1.22 g (6.23 mmol, yield 20%) of B-5.
References:
JP5688939,2015,B2 Location in patent:Paragraph 0142; 0146
