Lithium Hydroxide → 6-Methyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carboxylic acid

HRID 1260304노트

반응식

HRID 1260304 반응식
C([O:3][C:4]([C:6]1[C:11]([NH:12][C:13]2[CH:14]=[N:15][CH:16]=[N:17][CH:18]=2)=[N:10][CH:9]=[C:8]([CH3:19])[N:7]=1)=[O:5])C.[OH-].[Li+]>C1COCC1.C(O)C>[CH3:19][C:8]1[N:7]=[C:6]([C:4]([OH:5])=[O:3])[C:11]([NH:12][C:13]2[CH:18]=[N:17][CH:16]=[N:15][CH:14]=2)=[N:10][CH:9]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 673001846-Methyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carboxylic acid ethyl ester

생성물 1

HCID 583680556-Methyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carboxylic acid수율 69.6%

시약·촉매·용매 1

HCID 21873804Tetrahydrofuran ethanol용매

반응 조건

온도
0 °C

실험 절차

6-Methyl-3-(pyrimidin-5-ylamino)-pyrazine-2-carboxylic acid ethyl ester (300 mg, 1.15 mmol) was dissolved in a THF/ethanol (5 ml/1 ml) mixture, cooled to 0° C. and treated with lithium hydroxide (4.7 ml, 1N aqueous solution). The reaction mixture was allowed to warms to ambient temperature and stirred at that temperature for 1 hour. The pH value was subsequently adjusted to acidic and the resulting suspension was filtrated. The precipitate was washed with water and ethyl acetate and dried to yield the product as light yellow solid (185 mg, 69%).

후처리

  1. customwas allowed to warms to ambient temperature
  2. filtrationwas filtrated
  3. washThe precipitate was washed with water and ethyl acetate
  4. customdried

출처 및 근거

ORD 기록
ord-a5644691a59f43d2859a0ae977941b2b
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08470820B2

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