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ChemicalBook CAS DataBase List Methyl 4-(4-Boc-1-piperazinyl)-3-chlorobenzoate

Methyl 4-(4-Boc-1-piperazinyl)-3-chlorobenzoate synthesis

2synthesis methods
234082-35-0 Synthesis
3-Chloro-4-fluoro Methyl benzoate

234082-35-0
92 suppliers
$16.00/1g

57260-71-6 Synthesis
tert-Butyl 1-piperazinecarboxylate

57260-71-6
733 suppliers
$5.00/5g

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Yield:906559-46-4 74%

Reaction Conditions:

with potassium carbonate in dimethyl sulfoxide at 100; for 10 h;Sealed tube;

Steps:

2.2 Step-2

Methyl3-chloro-4-fluoro-benzoate (1.5 g, 7.9 mmol) was taken in a sealed tube, piperazine-1-carboxylic acid tert-butyl ester (1.48 g, 7.9 mmol) followed by K2C03 (3.29 g, 23 mmol)and DMSO (15 mL) were added and stirred at 100 °C for 10 h (TLC indicated completeconsumption of starting material). The reaction mixture was poured into ice-cold water (150mL) and extracted with EtOAc (2 x 100 mL). The combined organic extracts were washedwith brine (2 x 75 mL), dried over Na2S04 and concentrated under reduced pressure to givethe crude residue which was purified by column chromatography (100-200 silica gel, 30 g,10% EtOAc-hexane) to afford tert-butyl4-(2-chloro-4-methoxycarbonyl-phenyl)piperazinel-carboxylate (2.1 g, 74%) as a white solid LCMS: m/z: 355.4 [M+Ht.

References:

WO2018/125961,2018,A1 Location in patent:Page/Page column 30; 31

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