N,N-DIMETHYLAMINOMETHYLENEMALONIC ACID DIMETHYL ESTER synthesis
- Product Name:N,N-DIMETHYLAMINOMETHYLENEMALONIC ACID DIMETHYL ESTER
- CAS Number:18856-69-4
- Molecular formula:C8H13NO4
- Molecular Weight:187.19
Yield:18856-69-4 84%
Reaction Conditions:
in toluene at 100; for 5 h;Inert atmosphere;
Steps:
intermediate 26A: dimethyl 2-((dimethylamino)methyiene)malonate
To a solution of dimethyl malonate (10.00 g, 76.00 mmol) in toluene (100 mL) wasadded DMF-DMA (20.27 mL, 151.00 mmoi) at ambient temperature under a nitrogenatmosphere. The resulting reaction mixture was heated at 100°C for 5 h. The reaction mixture was cooled to ambient temperature and concentrated under reduced pressure to obtain intermediate 26A (13.00 g, 84.00%) as a yellow solid. ‘H NMR( 00 MIz, CDCI3) ppm 2.92 3.07 (m, 6 H), 3.66 3.72 (br.s., 3 H), 3.74 3.79 (br.s., 3 H), 7.53 (s, 1 H). LCMS (j’Vlethod-D):retention time 0,63 mm, [M±Hj 188.2. The compound was taken directly to the subsequent step without further purification or characterization.
References:
WO2018/93569,2018,A1 Location in patent:Page/Page column 103
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