N-(4-CYANO-PHENYL)-GLYCINE synthesis
- Product Name:N-(4-CYANO-PHENYL)-GLYCINE
- CAS Number:42288-26-6
- Molecular formula:C9H8N2O2
- Molecular Weight:176.17
Yield:42288-26-6 88%
Reaction Conditions:
in water at 100 - 110; for 3 h;
Steps:
3
3.2.3 Preparation of [(4-cyanophenyl)amino]acetic acid (V) C7H6N2 C2H3DPθ2 C9H8N2O2 MoI. Wt.: 1 18,14 MoI. Wt.: 138,95 MoI. Wt.: 176,17VIngredientsF: 90 g - 0.75 molG: 211.7 g - 1.5 molSodium bicarbonate: 35 g, 0.42 molThe starting substances F and G were mixed in 1250 ml of water and this suspension was inserted into a bath heated up to 100-110 0C. After three hours of heating the reaction container was removed from the bath, cooled in the fridge and the separated substance was sucked off. The substance was dried in a vacuum drier at the temperature of 100 °C. Yield: Crude product: 122 g (92.8%), HPLC: 97%The crude product was purified by conversion to the sodium salt and re-acidification using an aqueous solution of sodium bicarbonate. The acid was released by means of diluted hydrochloric acid (1 :1). After sucking off and washing with water the product was dried in a vacuum drier (105 °C). Yield: Purified product: 115 g (88%), HPLC: 99.1%, water content: 0.13%; sulphate ash: 1.8%
References:
ZENTIVA, K.S. WO2009/111997, 2009, A1 Location in patent:Page/Page column 11
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