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Sulfuric Acid → HCID 21568404、化合物

HRID 1579385
ノート
印刷プレビュー

反応式

HRID 1579385 の反応式
[Mg].[C:2]([O:10][CH2:11][CH3:12])(=[O:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[O:13]=[C:14]1[C:23]2[C:18](=[N:19][CH:20]=[CH:21][CH:22]=2)[O:17][C:16]2[CH:24]=[CH:25][C:26]([C:28](Cl)=[O:29])=[CH:27][C:15]1=2.S(=O)(=O)(O)O>O.C(O)C.ClC1C=CC=CC=1.C(Cl)(Cl)(Cl)Cl>[O:13]=[C:14]1[C:23]2[C:18](=[N:19][CH:20]=[CH:21][CH:22]=2)[O:17][C:16]2[CH:24]=[CH:25][C:26]([C:28]([CH:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])[C:2]([O:10][CH2:11][CH3:12])=[O:9])=[O:29])=[CH:27][C:15]1=2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 1118Sulfuric AcidHCID 7761Diethyl MalonateHCID 5462224MagnesiumHCID 53808777HCID 53808777、化合物

生成物 1

HCID 21568404HCID 21568404、化合物

試薬・触媒・溶媒 4

HCID 702Ethanol溶媒2 回
HCID 962
Water
溶媒
2 回
HCID 5943Carbon Tetrachloride溶媒
HCID 7964Chlorobenzene溶媒2 回

反応条件

温度
65 °C

実験手順

0.57 g of magnesium, 0.8 ml of carbon tetrachloride and 3.6 ml of absolute ethanol are placed in a four-necked flask fitted with a dropping funnel, a thermometer, a reflux condenser and a stirrer. 36.5 ml of chlorobenzene is added, and then a mixture of 2.67 g of diethyl malonate, 18 ml of chlorobenzene and 12.6 ml of absolute ethanol is added dropwise, while the temperature is maintained at 65°C. The mixture is allowed to stand at 85°C for 1 hour to complete the reaction. After cooling with water, 4 g of 5-oxo-5H-[1]benzopyrano[2,3-b]pyridine-7-carboxylic acid chloride is added, and the mixture is stirred at 30°-35°C for 1.5 hours. To the reaction mixture is added a mixture of 1 ml of concentrated sulfuric acid and 7 ml of water is added dropwise with stirring under ice cooling, and the precipitate (sodium sulfate) is removed by filtration. The residue is washed with water, dried, and concentrated. The residue is recrystallized from ethanol to give diethyl 2-(5-oxo-5H-[1]benzopyrano[2,3-b]pyridine- 7-yl-carbonyl)malonate as white crystals melting at 137°-138.5°C.

後処理

  1. customfitted with a dropping funnel
  2. additionis added dropwise, while the temperature
  3. customthe reaction
  4. additionis added
  5. additionTo the reaction mixture is added
  6. additionis added dropwise
  7. stirringwith stirring under ice cooling
  8. customthe precipitate (sodium sulfate) is removed by filtration
  9. washThe residue is washed with water
  10. customdried
  11. concentrationconcentrated
  12. customThe residue is recrystallized from ethanol

出典と根拠

ORDレコード
ord-f9d4cf9aa4bb400c86db9758784f499e
出典データセット
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03931199

反応ノート

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