methyl 4-(1,1-difluoroethyl)benzoate synthesis
- Product Name:methyl 4-(1,1-difluoroethyl)benzoate
- CAS Number:444915-84-8
- Molecular formula:C10H10F2O2
- Molecular Weight:200.18
3609-53-8
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Yield:444915-84-8 96%
Reaction Conditions:
with diethylamino-sulfur trifluoride in ethanol;chloroform at 80;Sealed tube;
Steps:
1.25.1 Step 1: methyl 4-(l,l-difluoroethyl)benzoate
Step 1: methyl 4-(l,l-difluoroethyl)benzoate [0254] To a solution of methyl 4-acetylbenzoate (5.0 g, 28 mmol) and DAST (11 mL, 84 mmol) in chloroform (15 mL) in a 50 mL pressure reaction tube was added EtOH (0.15 mL, 3.0 mmol). The resulting mixture was heated at 80°C overnight. After cooling to room temperature, the reaction mixture was poured into a saturated solution of NaHCO3 (150 mL), and then extracted with DCM. The organic layer was dried over sodium sulfate, filtered, and concentrated. The concentrate was purified by column chromatography over silica gel (hexane / ethyl acetate = 15:1) to afford the title compound as a colorless oil (5.4 g, 96%). *H NM (400 MHz, CDCI3) δ 8.10 (d, J = 8.4 Hz, 2H), 7.58 (d, J = 8.4 Hz, 2H), 3.94 (s, 3H), 1.93 (t, J = 18.0 Hz, 3H).
References:
WO2016/100349,2016,A2 Location in patent:Paragraph 0254
38078-09-0
370 suppliers
$15.00/1g
3609-53-8
198 suppliers
$5.00/1g
444915-84-8
15 suppliers
inquiry