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

HRID 864912ノート

反応式

HRID 864912 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]([OH:13])=O)=[C:6]([C:14]([OH:16])=[O:15])[N:5]=2>C(OC(=O)C)(=O)C>[CH3:1][C:2]1[O:3][C:4]2[C:9]([N:10]=1)=[CH:8][C:7]1[C:11]([O:16][C:14](=[O:15])[C:6]=1[N:5]=2)=[O:13]

参加物

3

反応物 1

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

生成物 1

HCID 153898982-Methyloxazolo[5,4-b]pyridine-5,6-dicarboxylic anhydride収率 97%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

反応条件

温度
70 °C

実験手順

A suspension of 2-methyloxazolo[5,4-b]pyridine-5,6-dicarboxylic acid (4.84 g, 0.0218 mol) in acetic anhydride (150 mL) is slowly heated to 70° C. at which point all the solids dissolve forming a yellow solution. The reaction mixture is heated at 70° C. overnight, cooled to room temperature, and concentrated in vacuo. Xylene is added to remove excess acetic anhydride by codistillation. 2-Methyloxazolo[5,4-b]pyridine-5,6-dicarboxylic anhydride is obtained as a pale yellow solid in 97% yield melting point 194°-196° C.

後処理

  1. dissolutiondissolve
  2. customforming a yellow solution
  3. temperatureThe reaction mixture is heated at 70° C. overnight
  4. temperaturecooled to room temperature
  5. concentrationconcentrated in vacuo
  6. additionXylene is added
  7. customto remove excess acetic anhydride by codistillation

出典と根拠

ORDレコード
ord-6b017c56843b41bb9a526586b3bfa6d2
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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