Quinolinic Acid → Furo[3,4-b]pyridine-5,7-dione

HRID 1054202

反応式

HRID 1054202 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([OH:9])=O)[C:2]=1[C:10]([OH:12])=[O:11].C(OC(=O)C)(=O)C>>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]2[C:7](=[O:9])[O:12][C:10](=[O:11])[C:2]=12

参加物

3

反応物 2

HCID 1066Quinolinic AcidHCID 7918Acetic Anhydride

生成物 1

HCID 69688Furo[3,4-b]pyridine-5,7-dione収率 86.7%

反応条件

温度
115 °C

実験手順

A mixture of pyridine-2,3-dicarboxylic acid (2 g, 12 mmol) and acetic anhydride was heated at 115° C. for 4 h. Excess reagent was removed under reduced pressure. The remaining solid was triturated with hot carbon tetrachloride. After cooling, the solid was collected by vacuum filtration and dried overnight under vacuum at 60° C. to give furo[3,4-b]pyridine-5,7-dione (1.55 g, 10.4 mmol). 1H NMR (400 MHz, DMSO-d6) δ 9.10 (dd, J=4.9, 1.5 Hz, 1H), 8.50 (dd, J=7.8, 1.5 Hz, 1H), 7.90 (dd, J=7.8, 4.9 Hz, 1H).

後処理

  1. customExcess reagent was removed under reduced pressure
  2. customThe remaining solid was triturated with hot carbon tetrachloride
  3. temperatureAfter cooling
  4. filtrationthe solid was collected by vacuum filtration
  5. customdried overnight under vacuum at 60° C.

出典と根拠

ORDレコード
ord-81551d410b3d4519b770d25cab2af8ed
出典データセット
uspto-grants-2016_07
特許番号
US09394299B2

関連ノート

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