Ethanol → HCID 135819170、化合物

HRID 1011423ノート

反応式

HRID 1011423 の反応式
[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([C:12]([OH:14])=[O:13])[CH:8]=[N:9]2)=[CH:4][CH:3]=1.O=S(Cl)Cl.O.C([O-])([O-])=O.[Na+].[Na+].[CH3:26][CH2:27]O>>[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([C:12]([O:14][CH2:26][CH3:27])=[O:13])[CH:8]=[N:9]2)=[CH:4][CH:3]=1

参加物

6

反応物 5

HCID 702EthanolHCID 962WaterHCID 10340Sodium CarbonateHCID 24386Thionyl ChlorideHCID 1361076117-Hydroxyquinoline-3-carboxylic acid

生成物 1

HCID 135819170HCID 135819170、化合物収率 64%

実験手順

To a solution of the compound obtained in stage A (15 g, 79 mmol) in EtOH (500 ml) was added dropwise SOCl2 (40 mL). The resulting mixture was stirred under reflux during 12 hours. After adding water (200 mL), the pH was adjusted to 7.0 with 20% aqueous Na2CO3. The aqueous solution was extracted with CH2Cl2 (3×200 mL). The combined organic layers were dried over MgSO4, filtered and evaporated to afford 11 g (yield: 64%) of the product of molecular formula C12H11NO3. Aspect: pale brown powder.

後処理

  1. temperatureunder reflux during 12 hours
  2. extractionThe aqueous solution was extracted with CH2Cl2 (3×200 mL)
  3. dry with materialThe combined organic layers were dried over MgSO4
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-906707339050480d8e32e713657091ad
出典データセット
uspto-grants-2011_07
特許番号
US07977354B2

反応ノート

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