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Phosphorus oxide (P4O10) → 3-Phenyl-7-propyl-1-benzofuran-6-ol

HRID 342763
ノート
印刷プレビュー

反応式

HRID 342763 の反応式
[CH2:1]([C:4]1[C:9]([O:10][CH2:11][C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=O)=[CH:8][CH:7]=[CH:6][C:5]=1[OH:20])[CH2:2][CH3:3].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>OP(O)(O)=O.O.CCOCC>[C:14]1([C:12]2[C:8]3[CH:7]=[CH:6][C:5]([OH:20])=[C:4]([CH2:1][CH2:2][CH3:3])[C:9]=3[O:10][CH:11]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 14812Phosphorus oxide (P4O10)HCID 543761242-Propyl-3-(2-phenyl-2-oxoethoxy)phenol

生成物 1

HCID 154629143-Phenyl-7-propyl-1-benzofuran-6-ol

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether触媒HCID 962Water溶媒HCID 1004Phosphoric Acid溶媒

実験手順

To a stirred suspension of 2-propyl-3-(2-phenyl-2-oxoethoxy)phenol (9.30 g) in o-phosphoric acid(85%) (93 mL) at room temperature was added over a 45 minutes period phosphorus pentoxide(46.50 g). During this period the reaction mixture was heated several times with a heat gun. After stirring the mixture for 30 minutes the reaction was checked by TLC(to take a little of sample with a capillary and dissolve sample in water and add several drops of ether; elution: 50% methylene chloride in hexane). The reaction mixture was heated again with heat gun if the reaction was not complete. The reaction mixture continued to be stirred for 20 minutes, then was poured into a beaker containing ice. The reaction flask was then rinsed with water and ether, and the washings were added to the beaker. The organic layer was separated, washed with water, dried over MgSO4, and concentrated. Column Chromatography (silica gel 60, 50% methylene chloride in hexane) gave the title compound.

後処理

  1. temperatureDuring this period the reaction mixture was heated several times with a heat gun
  2. washelution
  3. temperatureThe reaction mixture was heated again
  4. temperaturewith heat gun if the reaction
  5. stirringto be stirred for 20 minutes
  6. additionwas poured into a beaker
  7. additioncontaining ice
  8. washThe reaction flask was then rinsed with water and ether
  9. additionthe washings were added to the beaker
  10. customThe organic layer was separated
  11. washwashed with water
  12. dry with materialdried over MgSO4
  13. concentrationconcentrated

出典と根拠

ORDレコード
ord-217ca2d00562468ea793a75aa79840d8
出典データセット
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05859051

反応ノート

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