ChemicalBook CAS DataBase List 8-cyclopentyl-5-Methyl-2-(Methylthio)pyrido[2,3-d]pyriMidin-7(8H)-one

8-cyclopentyl-5-Methyl-2-(Methylthio)pyrido[2,3-d]pyriMidin-7(8H)-one synthesis

15synthesis methods

Product Name:8-cyclopentyl-5-Methyl-2-(Methylthio)pyrido[2,3-d]pyriMidin-7(8H)-one
CAS Number:362656-23-3
Molecular formula:C14H17N3OS
Molecular Weight:275.37

4-PyriMidinaMine, 5-broMo-N-cyclopentyl-2-(Methylthio)-

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8-cyclopentyl-5-Methyl-2-(Methylthio)pyrido[2,3-d]pyriMidin-7(8H)-one

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Yield:362656-23-3 86%

Reaction Conditions:

Stage #1: 5?bromo?N?cyclopentyl?2?(methylthio)pyrimidin?4?amine;(E)-but-2-enoic acidwith lead acetate;triethylamine in 1-methyl-pyrrolidin-2-one at 65; for 3.5 h;Inert atmosphere;
Stage #2: with lead acetate;acetic acid;triethylamine in 1-methyl-pyrrolidin-2-one at 65; for 8 h;Inert atmosphere;

Steps:

1.5 Example 1

Step 5, Preparation of 8-cyclopentyl-5-methyl-2-methylthiopyrido(2,3-d)pyrimidin-7(8H)-one:Take 287g of 5-bromo-4-cyclopentylamino-2-methylthiopyrimidine, add 800 ml of N-methylpyrrolidone, pass nitrogen gas for 30 min, add 200 mg of lead acetate,Nitrogen gas was bubbled for 30 minutes, 95g of crotonic acid and 220g of triethylamine were added, and nitrogen was bubbled for 30 minutes.The reaction was heated to 65° and the reaction was continued. After 2 hours, 200 mg of lead acetate was added for a total of three additional occasions. An additional 100 mg of acetic acid button was added at intervals of 2 hours.After a total of 8 hours of reaction, after the end of the reaction, the reaction was cooled to room humidity, 200 ml of acetic anhydride was added dropwise, and then the reaction was heated to 50 for 1 hour.After the end of the reaction, cool to room temperature, add water 1L, stir for one hour, suction filtration, filter cake washed with 500 ml of water,The solid was then beaten with 800 ml of isopropanol:water=1:1 mixed solvent, suction filtered, and the cake was dried under vacuum at 45° to give 236 g of a white powdery solid, yield 86%;

References:

CN107488175,2017,A Location in patent:Paragraph 0009; 0010

362656-11-9 Synthesis