ChemicalBook CAS DataBase List 3-Hydroxyphenylphosphinyl-propanoic acid

3-Hydroxyphenylphosphinyl-propanoic acid synthesis

4synthesis methods

Product Name:3-Hydroxyphenylphosphinyl-propanoic acid
CAS Number:14657-64-8
Molecular formula:C9H11O4P
Molecular Weight:214.15

644-97-3

79-10-7

3-Hydroxyphenylphosphinyl-propanoic acid

14657-64-8

Method of preparing waste water-free 2-carboxyethylphenyl hypophosphite according to the present invention, with the following steps: (1) adding 1.0 mol of dichlorophenylphosphine to a reaction vessel, stirring and heating to 80°C, then adding 1 mol of acrylic acid drop by drop, followed by raising the temperature to 110°C, maintaining the reaction at this temperature for 3 hours, and then cooling down to 50°C after completion of the reaction; (2) adding to the reaction solution obtained in step (1) 2.0 mol dichloropropane (secondary use of mother liquor, material supplement), stir thoroughly; (3) slowly add 1.0 mol water dropwise to the mixture of step (2) under stirring to carry out the hydrolysis reaction of the chlorine chloride intermediate, after the dropwise addition is completed, heat to 90 ℃, maintain for 3 hours, and then cooled to 20 ℃, to generate 2-carboxyethyl phenyl phosphinic acid, and to recover hydrochloric acid as a by-product; (4) the solid-liquid mixture obtained from step (3) is subjected to the following reaction ) the solid-liquid mixture obtained in step (3) was filtered, and the solid was washed with dichloropropane, and after filtering again, the solid was placed in an oven and baked at 130°C for 2 hrs to obtain 2-carboxyethylphenyl hypophosphite, and the mother liquor was recovered in the next batch of production. 2-carboxyethylphenyl hypophosphite showed a yield of 98.0%, a melting point of 160.2°C, an acid value (mgKOH/g) of 522, and a phosphorus content of 14.35%, and the product quality was excellent.

644-97-3
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$14.00/5g

79-10-7 Synthesis

79-10-7
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$20.16/100 mL

14657-64-8
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$5.00/1g

Yield:14657-64-8 98%

Reaction Conditions:

Stage #1:Dichlorophenylphosphine;acrylic acid at 80 - 110; for 3 h;
Stage #2: with water at 90; for 3 h;Temperature;Concentration;

Steps:

5.1; 5.2; 5.3; 5.4 Example 5 A process for the production of 2-carboxyethylphenylphosphinic acid with no waste water as mentioned in the present invention.
A process for the production of 2-carboxyethylphenylphosphinic acid in accordance with the present invention without waste water,Next:(1) 1.0 mol of phenylphosphine dichloride was charged into a reaction vessel, stirred, heated to 80 ° C, 1 mol of acrylic acid was added dropwise,Finished warming to 110 deg C , heat 3 hours, cooling to 50 deg C ; (2) To the liquid obtained in the step (1), 2.0 mol of dichloropropane (secondary used mother liquor,Material complement), stirring;(3) to the step (2) to slowly drop 1.0mol of water, acid chloride intermediates and water hydrolysis reaction, drop finishedHeating to 90 DEG C, keeping for 3 hours, cooling to 20 DEG C to produce 2-carboxyethylphenylphosphinic acid, and recovering by-product hydrochloric acid.(4) The solid-liquid mixture obtained in step (3) was filtered, washed with dichloropropane, filtered again, placed in an oven,Baking at 130 ° C for 2 hours to obtain 2-carboxyethylphenylphosphinic acid, and the mother liquor was recovered in the next batch. The yield of 2-carboxyethylphenylphosphinic acid was 98.0%, the melting point was 160.2 deg C , the acid value (mgKOH / g) was 522, the phosphorus content was 14.35%, and the product quality was excellent.

References:

Dongying Merida new materials Technology Co., Ltd;Zhang, Guixin;Guo, Qing;Zhang, Hua CN105541908, 2016, A Location in patent:Paragraph 0023; 0024

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