Process of preparing (s)-2-(2-carbonyl-tetrahydropyrimidyl-1-(2H)-3-methyl butyric acid

Process of preparing (s)-2-(2-carbonyl-tetrahydropyrimidyl-1-(2H)-3-methyl butyric acid

  • CN 101,088,991 A
  • Filed: 06/12/2006
  • Published: 12/19/2007
  • Est. Priority Date: 06/12/2006
  • Status: Active Application
First Claim
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1. (S)-3 methyl-2-(the butyro-preparation method of 2-carbonyl-tetrahydropyrimidine-1 (2H)-yl) may further comprise the steps:

  • (1) in the presence of alkali, (S)-2-amido-3 Methylbutanoic acid and vinyl cyanide in water in 0~

    50 ℃

    of reaction 6~

    24 hours, acidified and aftertreatment obtains (S)-2-(2-cyano group ethylamino-)-3 Methylbutanoic acid, described vinyl cyanide with (S)-equivalence ratio of 2-amido-3 Methylbutanoic acid is 1;

    1;

    (2) under the existence and RaneyNi catalytic condition of alkali, feeding ammonia to pressure in the solvent that contains (S)-2-(2-cyano group ethylamino-)-3 Methylbutanoic acid is 0.1MPa~

    0.8MPa, feeding hydrogen to total pressure then is 0.2~

    4.0MPa, 20~

    100 ℃

    of reactions 24~

    80 hours, acidified and aftertreatment obtains (S)-2-(3-amido Propylamino)-3 Methylbutanoic acid, and described solvent is water or C 1-C 8Alcoholic solvent or its mixture;

    (3) in the presence of alkali, (S)-2-(3-amido Propylamino)-3 Methylbutanoic acid and triphosgene or two phosgene in solvent in 0~

    40 ℃

    of reaction 1 hour, acidified and aftertreatment obtains (S)-3-methyl-2-(2-carbonyl-tetrahydropyrimidine-1 (2H)-yl) butyric acid, the equivalence ratio of described (S)-2-(3-amido Propylamino)-3 Methylbutanoic acid and triphosgene or two phosgene is 1~

    3;

    3, and described solvent is water or organic solvent or its mixture.

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