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

HRID 1260304ノート

反応式

HRID 1260304 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 21873804Tetrahydrofuran ethanol溶媒

反応条件

温度
0 °C

実験手順

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%).

後処理

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

出典と根拠

ORDレコード
ord-a5644691a59f43d2859a0ae977941b2b
出典データセット
uspto-grants-2013_06
特許番号
US08470820B2

反応ノート

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