3,4-dihydro-2H-pyran → 2-(3-iodopropoxy)tetrahydro-2H-pyran

HRID 652461

反応式

HRID 652461 の反応式
[I:1][CH2:2][CH2:3][CH2:4][OH:5].[O:6]1[CH:11]=[CH:10][CH2:9][CH2:8][CH2:7]1.C1C=CC(N=NC2C=CC(N)=NC=2N)=CC=1.Cl.CC1C=CC(S(O)(=O)=O)=CC=1>ClCCl>[I:1][CH2:2][CH2:3][CH2:4][O:5][CH:7]1[CH2:8][CH2:9][CH2:10][CH2:11][O:6]1

参加物

5

実験手順

A solution of 3-iodopropanol (15 g, 80.65 mole), dihydropyran (14.7 ml, 161.29 mole) and pyridium p-toluenesulfonate (500 g, 2.0 mole) in 100 ml of dry dichloromethane was stirred at room temperature under an atmosphere of nitrogen for 2.5 hours. The resulting mixture was diluted with dichloromethane (150 ml), washed with water and a saturated sodium bicarbonate solution, dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue was flash chromatographed on a silica gel to give 20.43 g of the title A compound as an oil.

後処理

  1. washwashed with water
  2. dry with materiala saturated sodium bicarbonate solution, dried over anhydrous magnesium sulfate
  3. customevaporated in vacuo
  4. customchromatographed on a silica gel

出典と根拠

ORDレコード
ord-39108c3189d14463b393a5bf0ef51f59
出典データセット
uspto-grants-1987_06
特許番号
US04672075

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