Malonic Acid → HCID 20517749、化合物

HRID 2198878ノート

反応式

HRID 2198878 の反応式
[C:1]([OH:4])(=[O:3])[CH3:2].O[C:6]1[CH:19]=[C:18]2[C:9]([CH:10]=[CH:11][C:12]3[O:13][CH:14]=[C:15](C=O)[C:16](=[O:20])[C:17]=32)=[CH:8][CH:7]=1.[C:23](O)(=O)[CH2:24][C:25]([OH:27])=[O:26]>N1C=CC=CC=1>[C:1]([O:4][C:6]1[CH:19]=[C:18]2[C:9]([CH:10]=[CH:11][C:12]3[O:13][CH:14]=[C:15]([C:24](=[CH2:23])[C:25]([OH:27])=[O:26])[C:16](=[O:20])[C:17]=32)=[CH:8][CH:7]=1)(=[O:3])[CH3:2]

参加物

4

反応物 2

HCID 867Malonic Acid2 回HCID 867372399-hydroxy-1-oxo-1H-naphtho[2,1-b]pyran-2-carboxaldehyde acetate

生成物 1

HCID 20517749HCID 20517749、化合物収率 25.5%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mixture of 9-hydroxy-1-oxo-1H-naphtho[2,1-b]pyran-2-carboxaldehyde acetate (10.0 g, 0.0354 m) and malonic acid (4.0 g, 0.0354 m) in pyridine (100 ml) is refluxed for 45 minutes. Additional malonic acid (1.0 g, 0.00885 m, 0.25 eq.) is added and the reaction refluxed for 30 minutes. The solvent is removed under reduced pressure to give a sludge from which product crystallizes on the addition of acetone. After filtering the product, recrystallization from DMF gives cocoa crystals (2.75 g, 24%), m.p. dec>290° C.

後処理

  1. temperatureis refluxed for 45 minutes
  2. temperaturethe reaction refluxed for 30 minutes
  3. customThe solvent is removed under reduced pressure
  4. customto give a sludge from which product
  5. customcrystallizes on the addition of acetone
  6. filtrationAfter filtering
  7. customthe product, recrystallization from DMF

出典と根拠

ORDレコード
ord-e4e8062f30fa48399586d60bb6ab6171
出典データセット
uspto-grants-1982_11
特許番号
US04360527

反応ノート

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