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

HRID 1947710ノート

反応式

HRID 1947710 の反応式
[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

参加物

7

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f74fef564e6d4da583fd4e4cc8340286
出典データセット
uspto-grants-2013_03
特許番号
US08399480B2

反応ノート

読み込み中…