Sulfuric Acid → HCID 86639059、化合物

HRID 1690056ノート

反応式

HRID 1690056 の反応式
S(=O)(=O)(O)O.[F:6][C:7]([F:21])([F:20])[C:8]1[N:13]=[C:12]2[CH:14]=[C:15]([C:17]([OH:19])=[O:18])[NH:16][C:11]2=[CH:10][CH:9]=1>C(O)C>[F:21][C:7]([F:6])([F:20])[C:8]1[N:13]=[C:12]2[CH:14]=[CH:15][NH:16][C:11]2=[CH:10][CH:9]=1.[CH3:14][CH2:15][C:17]([O-:19])=[O:18]

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 573558695-(Trifluoromethyl)-1H-pyrrolo[3,2-b]pyridine-2-carboxylic acid

生成物 1

HCID 86639059HCID 86639059、化合物収率 168.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1 mL (18.71 mmol) of concentrated sulfuric acid is added to a solution of 0.2 g (0.87 mmol) of 5-trifluoromethyl-pyrrolo[3,2-b]pyridine-2-carboxylic acid, obtained in Stage 10.2, in 10 mL of ethanol. It is stirred under reflux for 20 hours then the solution is cooled, and concentrated at reduced pressure. The resultant residue is then taken up in 50 mL of dichloromethane then washed successively with 20 mL of a saturated aqueous solution of sodium bicarbonate, 40 mL of water and 20 mL of saturated aqueous solution of sodium chloride, dried over sodium sulfate and then concentrated at reduced pressure. We obtain 0.19 g of product, which is used as it is in the next stage.

後処理

  1. temperatureunder reflux for 20 hours
  2. temperaturethe solution is cooled
  3. concentrationconcentrated at reduced pressure
  4. washthen washed successively with 20 mL of a saturated aqueous solution of sodium bicarbonate, 40 mL of water and 20 mL of saturated aqueous solution of sodium chloride
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated at reduced pressure

出典と根拠

ORDレコード
ord-b82352c8274a47799e4a9686a753c9ed
出典データセット
uspto-grants-2012_04
特許番号
US08153650B2

反応ノート

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