Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → 6-(2-hydroxyethyl)-6H-furo[2,3-c]pyridin-7-one

HRID 1183078ノート

反応式

HRID 1183078 の反応式
C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1.O1CCCCC1[O:24][CH2:25][CH2:26][N:27]1[CH:32]=[CH:31][C:30]2[CH:33]=[CH:34][O:35][C:29]=2[C:28]1=[O:36].C(=O)([O-])O.[Na+]>CO>[OH:24][CH2:25][CH2:26][N:27]1[CH:32]=[CH:31][C:30]2[CH:33]=[CH:34][O:35][C:29]=2[C:28]1=[O:36]

参加物

5

反応物 3

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 516892Sodium BicarbonateHCID 686754816-[2-(tetrahydropyran-2-yloxy)ethyl]-6H-furo[2,3-c]pyridin-7-one

生成物 1

HCID 686744936-(2-hydroxyethyl)-6H-furo[2,3-c]pyridin-7-one収率 73.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Pyridinium p-toluenesulfonate (0.21 g, 0.85 mmol) was added to a methanol solution (20 ml) of 6-[2-(tetrahydropyran-2-yloxy)ethyl]-6H-furo[2,3-c]pyridin-7-one (0.45 g, 1.7 mmol), and stirred at room temperature for 2 days. An aqueous sodium hydrogen carbonate solution was added to the reaction mixture, and extracted with dichloromethane. The organic layer was dried over anhydrous sodium sulfate, and concentrated under reduced pressure. Diethyl ether was added to the residue to precipitate crystals. The crystals were collected by filtration and dried to thereby obtain 223 mg (yield: 73%) of 6-(2-hydroxyethyl)-6H-furo[2,3-c]pyridin-7-one as a white powder.

後処理

  1. extractionextracted with dichloromethane
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. additionDiethyl ether was added to the residue
  5. customto precipitate crystals
  6. filtrationThe crystals were collected by filtration
  7. customdried

出典と根拠

ORDレコード
ord-49eeb06c8f03415daca202c7a1e0af81
出典データセット
uspto-grants-2014_03
特許番号
US08664217B2

反応ノート

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