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

HRID 467748노트

반응식

HRID 467748 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)=[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-cb4497fe369c4281a791a9fdb83fbe53
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623866B2

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