3,4-dihydro-2H-pyran → Diethyl 5-(tetrahydropyran-2-yloxy)pentylphosphonate

HRID 2013

反応式

HRID 2013 の反応式
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][P:7](=[O:14])([O:11][CH2:12][CH3:13])[O:8][CH2:9][CH3:10].[O:15]1[CH:20]=[CH:19][CH2:18][CH2:17][CH2:16]1.C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1>ClCCl>[O:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]1[O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][P:7](=[O:14])([O:8][CH2:9][CH3:10])[O:11][CH2:12][CH3:13]

参加物

5

反応物 3

HCID 80803,4-dihydro-2H-pyranHCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 10680635Diethyl 5-hydroxypentylphosphonate

生成物 1

HCID 19689209Diethyl 5-(tetrahydropyran-2-yloxy)pentylphosphonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 66.9 g (0.298 mol) of diethyl 5-hydroxypentylphosphonate, 32.6 g (0.38 mol) of 3,4-dihydropyran and 1 g (0.004 mol) of pyridinium toluene-4-sulfonate in 800 ml of dichloromethane was heated under reflux for 16 hours. The solution was washed with water and saturated sodium hydrogen carbonate solution, dried over sodium sulfate and distilled in a bulb tube.

後処理

  1. temperatureunder reflux for 16 hours
  2. washThe solution was washed with water and saturated sodium hydrogen carbonate solution
  3. dry with materialdried over sodium sulfate
  4. distillationdistilled in a bulb tube

出典と根拠

ORDレコード
ord-1e24e4dd0b0641159e1602ba6f4a336e
出典データセット
uspto-grants-1998_03
特許番号
US05728686

関連ノート

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