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

HRID 54187노트

반응식

HRID 54187 반응식
[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]

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a620016f604b4c2598b0e4d156448e73
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05622913

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