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Ethyl 3-hydroxyfuro[3,2-c]pyridine-2-carboxylate → Furo[3,2-c]pyridin-3(2H)-one

HRID 1984291
ノート
印刷プレビュー

反応式

HRID 1984291 の反応式
[OH:1][C:2]1[C:6]2[CH:7]=[N:8][CH:9]=[CH:10][C:5]=2[O:4][C:3]=1C(OCC)=O>Cl>[O:4]1[C:5]2[CH:10]=[CH:9][N:8]=[CH:7][C:6]=2[C:2](=[O:1])[CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 54695711Ethyl 3-hydroxyfuro[3,2-c]pyridine-2-carboxylate

生成物 1

HCID 14199081Furo[3,2-c]pyridin-3(2H)-one収率 15.1%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

Ethyl 3-hydroxyfuro[3,2-c]pyridine-2-carboxylate (5.79 g, 27.9 mmol) was dissolved in 10% hydrochloric acid (50 mL), and heated under reflux for 40 h. The reaction mixture was evaporated to dryness. The residue was suspended in saturated sodium bicarbonate solution and extracted with chloroform 3 times. The chloroform extracts were combined, dried (MgSO4), filtered, and evaporated to give furo[3,2-c]pyridin-3(2H)-one (570 mg) as a light-brown oil. N,N-Diisopropylethylamine (616 mg, 4.77 mmol) was added slowly to a solution of furo[3,2-c]pyridin-3(2H)-one (560 mg, 4.14 mmol) in dry methylene chloride (25 mL) under nitrogen at −10° C. Then trifluoromethanesulfonic anhydride (1.40 g, 4.97 mmol) was added slowly. The mixture was allowed to warm to RT, and stirred for another 1 g. The reaction was quenched with water. The organic layer was washed with water, dried (MgSO4), filtered, and then the solvent was evaporated to give the sub-title compound as a brown oily residue (1.10 g), which was used without further purification for the next step.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 40 h
  3. customThe reaction mixture was evaporated to dryness
  4. extractionextracted with chloroform 3 times
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated

出典と根拠

ORDレコード
ord-b94f9a55e53b4a789ee44185f2992ecf
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07544693B2

反応ノート

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