Dimethyl 2-(4-(methylsulfonyl)-2-nitrophenyl)malonate synthesis
- Product Name:Dimethyl 2-(4-(methylsulfonyl)-2-nitrophenyl)malonate
- CAS Number:917562-22-2
- Molecular formula:C12H13NO8S
- Molecular Weight:331.3
97-07-4
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917562-22-2
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$45.00/100mg
Yield:917562-22-2 100%
Reaction Conditions:
Stage #1: malonic acid dimethyl esterwith potassium tert-butylate in tert-butyl alcohol;
Stage #2: 1-chloro-4-methanesulfonyl-2-nitrobenzene in tert-butyl alcohol at 20; for 15 h;Heating / reflux;
Steps:
85.A
To a solution of KOtBu (17.1 mL, 17.1 mmol) in t-BuOH (10 mL) was added dropwise dimethyl malonate (2.0 mL, 17.1 mmol). To the resulting mixture was added a warm solution of 1-chloro-4-(methylsulfonyl) 2-nitrobenzene (2.0 g, 8.6 mmol) in t-BuOH (10 mL). The reaction mixture was heated at reflux for 15 h, then was cooled to RT and diluted with EtOAc (50 mL), washed with water and brine (30 mL each), dried (MgSO4) and concentrated in vacuo to provide Part A compound (2.8 g, 100%).
References:
US2008/9465,2008,A1 Location in patent:Page/Page column 91