3-CHLOROMETHYL-4-METHOXY-BENZOIC ACID METHYL ESTER synthesis
- Product Name:3-CHLOROMETHYL-4-METHOXY-BENZOIC ACID METHYL ESTER
- CAS Number:36755-02-9
- Molecular formula:C10H11ClO3
- Molecular Weight:214.65
77670-42-9
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18107-18-1
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36755-02-9
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Yield:36755-02-9 98%
Reaction Conditions:
in methanol;dichloromethane at 0 - 20; for 0.5 h;
Steps:
methyl 3-(chloromethyl)-4-methoxybenzoate
A cold (0° C. ice bath) solution of 3-(chloromethyl)-4-methoxybenzoic acid (0.465 g, 2.318 mmol) in dry dichloromethane (1.5 mL) and methanol (1.5 mL) was treated with TMS-Diazomethane (5.79 mL, 11.59 mmol). The mixture was stirred for 10 minutes, then warmed to room temperature and stirred for 20 minutes. The reaction was concentrated under reduced pressure, dried twice from dichloromethane, then dried under vacuum for 20 minutes to afford the product (0.490 g, 2.283 mmol, 98% yield) as a white powder. LCMS (Condition ACN-TFA, ES+) M+H=215.1, 0.92 minutes, calculated exact mass=214.04. 1H NMR (400 MHz, CDCl3) δ: 8.07 (d, J=2.3 Hz, 1H), 8.03 (dd, J=8.5, 2.3 Hz, 1H), 6.93 (d, J=8.5 Hz, 1H), 4.66 (s, 2H), 3.95 (s, 3H), 3.90 (s, 3H).
References:
US2015/291549,2015,A1 Location in patent:Paragraph 1163; 1164
38870-89-2
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121-98-2
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36755-02-9
21 suppliers
$90.00/100mg