METHYL 2-CHLORO-4-FLUORO-5-NITROBENZOATE synthesis
- Product Name:METHYL 2-CHLORO-4-FLUORO-5-NITROBENZOATE
- CAS Number:85953-30-6
- Molecular formula:C8H5ClFNO4
- Molecular Weight:233.58
67-56-1
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114776-15-7
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85953-30-6
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$90.00/1g
Yield:85953-30-6 67%
Reaction Conditions:
Stage #1: methanol;2-chloro-4-fluoro-5-nitrobenzoic acidwith sulfuric acid at 65; for 4 h;
Stage #2: at 65; for 3 h;Molecular sieve;
Steps:
1 Step 1: Synthesis of methyl 2-chloro-4-fluoro-5-nitrobenzoate (intermediate III -01')
To a stirred solution of 2-chloro-4-fluoro-5-nitrobenzoic acid (9.93 g, 45.23 mmol) in MeOH (100 mL) was added sulfuric acid (2.5 ml, 46.9 mmol). The reaction mixture was stirred at 65°C for 4 h, molecular sieves were added, and the reaction stirred at 65°C for further 3 h. The reaction mixture was filtered through Celiteto remove sieves, then concentrated under reduced pressure. The residue was taken up into DCM (200 mL), washed with water (150 mL). The aqueous was further extracted with DCM (4x 100 mL). The combined organic phases were washed with aqueous saturated NaHC03solution (2x 150 mL), brine (150 mL), and dried over MgS04, filtered andconcentrated under reduced pressure to afford 7.12 g of the desired product as a pale yellow solid in 67% yield and in 99% purity
References:
JP2018/508527,2018,A Location in patent:Paragraph 0218; 0219
85953-29-3
173 suppliers
$6.00/1g
85953-30-6
47 suppliers
$90.00/1g
114776-15-7
195 suppliers
$9.00/1g
85953-30-6
47 suppliers
$90.00/1g