METHYL BROMODIFLUOROACETATE synthesis
- Product Name:METHYL BROMODIFLUOROACETATE
- CAS Number:683-98-7
- Molecular formula:C3H3BrF2O2
- Molecular Weight:188.96
Yield:683-98-7 17.7 g
Reaction Conditions:
with ozone in dichloromethane at 20; under 760.051 Torr; for 3 h;
Steps:
1 Preparation of methyl bromide difluoroacetate
At room temperature and pressure,A solution of difluorodichlorodibromoethane (30 g, 0.1 mol)Methanol (32 g, 1.0 mol), dichloromethane (120 g, 1.4 mol)Adding to a reactor equipped with a condenser tube,Open the ozone generator,Ozone flow rate 6g / h. After 3 hours,The reaction solution was washed with water,Saturated sodium bisulfite,Saturated sodium bicarbonate,Organic layer added 15g methanol,Continue to react to the conversion of raw materials,Then again with water,Saturated sodium bisulfite,Saturated sodium bicarbonate,Saturated brine washing,The organic layer was dried over anhydrous magnesium sulfate,To obtain the crude bromo difluoroacetate,The resulting crude product was transferred to a distillation column for distillation,A fraction of 94 ° C to 96 ° C was collected,And finally 17.7 g of methyl bromide difluoroacetate, the molar yield was 92%.
References:
LIANYUANGANG JINKANG PHARMACEUTICAL TECHNOLOGY CO., LTD.;CHENG, YONGZHI;WANG, HAI;JI, LI CN104628559, 2017, B Location in patent:Paragraph 0078-0080
3222-05-7
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$154.34/1G
683-98-7
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$16.00/1g
