Lithium iodide → 2,3,5,6-Tetrahydro-3-(2-methoxy)ethylthiopyran-4-one

HRID 1381687ノート

反応式

HRID 1381687 の反応式
C([C:5]1([CH2:12][CH2:13][O:14][CH3:15])[C:10](=[O:11])[CH2:9][CH2:8][S:7][CH2:6]1)(OC)=O.[I-].[Li+].O.Cl>CN(C=O)C>[CH3:15][O:14][CH2:13][CH2:12][CH:5]1[C:10](=[O:11])[CH2:9][CH2:8][S:7][CH2:6]1

参加物

5

反応物 3

HCID 66321Lithium iodideHCID 21276494HCID 21276494、化合物HCID 21885828Hydrate;hydrochloride

生成物 1

HCID 212765012,3,5,6-Tetrahydro-3-(2-methoxy)ethylthiopyran-4-one収率 50.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2.4 g (10.3 mmol) of product from Step A in 50 ml DMF was added 6 g (44.8 mmol) lithium iodide. The resulting solution was refluxed under N2 for 2 hours. The reaction mixture was poured into 500 ml H2O/HCl and extracted with ethyl acetate. THe organic solution was washed with water; saturated NaCl, dried over MgSO4 and concentrated in vacuo to give 1.7 g crude product which was chromatographed through a pressure column eluting with 10% ethyl acetate/n-hexane to give 0.9 g of title compound.

後処理

  1. temperatureThe resulting solution was refluxed under N2 for 2 hours
  2. extractionextracted with ethyl acetate
  3. washTHe organic solution was washed with water
  4. dry with materialsaturated NaCl, dried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customto give 1.7 g crude product which
  7. customwas chromatographed through a pressure column
  8. washeluting with 10% ethyl acetate/n-hexane

出典と根拠

ORDレコード
ord-bde03a1913b746bfa68127fc4b3b23db
出典データセット
uspto-grants-1989_02
特許番号
US04803286

反応ノート

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