TERT-BUTYL 2-CHLORO-5-NITROBENZOATE synthesis
- Product Name:TERT-BUTYL 2-CHLORO-5-NITROBENZOATE
- CAS Number:55233-05-1
- Molecular formula:C11H12ClNO4
- Molecular Weight:257.67
2516-96-3
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Yield:55233-05-1 85%
Reaction Conditions:
Stage #1: 2-chloro-5-nitrobenzoic acidwith thionyl chloride;N,N-dimethyl-formamide in toluene; for 1.5 h;Heating / reflux;
Stage #2: potassium tert-butylate in tetrahydrofuran at 0; for 0.5 h;
Steps:
A
2-Chloro-5-nitrobenzoic acid (22 g, 109.1 mmol) and DMF (500 μL) are refluxed in toluene (50 mL)/thionyl chloride (8.5 mL) for 1.5 h with stirring. The reaction mixture is evaporated down and the residue is taken up in anhydrous THF (200 mL). Potassium- tert.- butoxide (12.5 g, 111.4 mmol) is added at 0 0C, then the cooling is removed and the mixture is stirred for 30 min The solvent is distilled off and the residue is divided between water and EtOAc. The organic phase is washed with water and 0.1 N NaOH, dried, filtered and evaporated down. Yield: 24 g (85 %)
References:
WO2008/152013,2008,A1 Location in patent:Page/Page column 15
2516-96-3
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55233-05-1
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25784-91-2
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$39.00/5G
865-47-4
658 suppliers
$14.00/25ML
55233-05-1
21 suppliers
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