Lithium Hydroxide → [4-Methyl-6-oxopyridazin-1(6H)-yl]acetic acid

HRID 243679노트

반응식

HRID 243679 반응식
[CH3:1][C:2]1[CH:3]=[N:4][N:5]([CH2:9][C:10]([O:12]CC)=[O:11])[C:6](=[O:8])[CH:7]=1.[OH-].[Li+].FC(F)(F)C(O)=O>O1CCCC1.CO.O>[CH3:1][C:2]1[CH:3]=[N:4][N:5]([CH2:9][C:10]([OH:12])=[O:11])[C:6](=[O:8])[CH:7]=1

참가 물질

7

반응물 3

HCID 3939Lithium HydroxideHCID 6422Trifluoroacetic acidHCID 77231410ethyl [4-methyl-6-oxopyridazin-1(6H)-yl]acetate

생성물 1

HCID 66939440[4-Methyl-6-oxopyridazin-1(6H)-yl]acetic acid

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To ethyl [4-methyl-6-oxopyridazin-1(6H)-yl]acetate (0.575 g, 2.93 mmol) in tetrahydrofuran (3 mL), methanol (2 mL) and water (2 mL) was added 1 N lithium hydroxide solution (2.9 mL). The reaction mixture was stirred at ambient temperature for 1.5 h. After neutralized with trifluoro acetic acid, the reaction mixture was directly purified by reverse phase HPLC (TMC Pro-Pac C18; 0-45% 0.1% trifluoroacetic acid in acetonitrile/0.1% trifluoroacetic acid in water gradient). The pure fractions were lyophilized overnight to yield the title compound. LC/MS 169.2 (M+1).

후처리

  1. customthe reaction mixture was directly purified by reverse phase HPLC (TMC Pro-Pac C18; 0-45% 0.1% trifluoroacetic acid in acetonitrile/0.1% trifluoroacetic acid in water gradient)
  2. waitThe pure fractions were lyophilized overnight

출처 및 근거

ORD 기록
ord-a7ab1ae7264346d0bf61f3e558d1581c
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653260B2

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