Hydrochloric Acid → 6-Chloro-3-(pyrimidin-5-ylamino)-pyridine-2-carboxylic acid

HRID 467748ノート

反応式

HRID 467748 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)=[CH:10][CH:9]=[C:8]([Cl:19])[N:7]=1)=[O:5])C.[Li+].[OH-].Cl>C1COCC1.C(O)C>[Cl: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)=[CH:10][CH:9]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 866601932-Pyridinecarboxylic acid, 6-chloro-3-(5-pyrimidinylamino)-, ethyl ester

生成物 1

HCID 866601946-Chloro-3-(pyrimidin-5-ylamino)-pyridine-2-carboxylic acid

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

A suspension of 6-chloro-3-(pyrimidin-5-ylamino)-pyridine-2-carboxylic acid ethyl ester (98 mg, 0.35 mmol) in THF (1 ml) and ethanol (0.5 ml) was cooled to 0° C. and treated with 1M LiOH (0.7 ml, 0.7 mmol). The ice bath was removed and the reaction mixture was stirred at rt. for 2 h. 1M HCl (0.7 ml, 0.7 mmol) was added and stirring was continued until a precipitate was forming. The reaction mixture was sucked off and the product was obtained upon drying of the precipitate as yellow solid (60 mg, 67%).

後処理

  1. customThe ice bath was removed
  2. stirringstirring
  3. customwas forming
  4. customthe product was obtained
  5. dry with materialupon drying of the precipitate as yellow solid (60 mg, 67%)

出典と根拠

ORDレコード
ord-cb4497fe369c4281a791a9fdb83fbe53
出典データセット
uspto-grants-2014_01
特許番号
US08623866B2

反応ノート

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