Sodium Hydroxide → 2-Methyloxazolo[5,4-b]pyridine-5,6-dicarboxylic acid

HRID 864911ノート

反応式

HRID 864911 の反応式
[CH3:1][C:2]1[O:3][C:4]2[C:9]([N:10]=1)=[CH:8][C:7]([C:11]([O:13]CC)=[O:12])=[C:6]([C:16]([O:18]CC)=[O:17])[N:5]=2.[OH-].[Na+]>CO.O>[CH3:1][C:2]1[O:3][C:4]2[C:9]([N:10]=1)=[CH:8][C:7]([C:11]([OH:13])=[O:12])=[C:6]([C:16]([OH:18])=[O:17])[N:5]=2

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 19958238Diethyl 2-methyloxazolo[5,4-b]pyridine-5,6-dicarboxylate

生成物 1

HCID 199581932-Methyloxazolo[5,4-b]pyridine-5,6-dicarboxylic acid収率 61%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of diethyl 2-methyloxazolo[5,4-b]pyridine-5,6-dicarboxylate (5.42 g, 0.0195 mol) dissolved in absolute methanol (160 mL) is added a 10% aqueous sodium hydroxide solution (36.1 mL, 0.0974 mol). A white precipitate slowly forms. The reaction is stirred at room temperature for one hour, diluted with water (20 mL) to dissolve the precipitate, and concentrated in vacuo. The residue is dissolved in water and acidified to pH 2-3 with concentrated HCl. The resulting white precipitate is collected by filtration, washed with water, and air dried to give 2-methyloxazolo[5,4-b]pyridine-5,6-dicarboxylic acid in 61% yield, melting point 235°-236° C. (dec).

後処理

  1. dissolutionto dissolve the precipitate
  2. concentrationconcentrated in vacuo
  3. dissolutionThe residue is dissolved in water
  4. filtrationThe resulting white precipitate is collected by filtration
  5. washwashed with water, and air
  6. customdried

出典と根拠

ORDレコード
ord-fba5919324884d90bc59e7a2e5d0a0e3
出典データセット
uspto-grants-1996_10
特許番号
US05565411

反応ノート

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