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

HRID 342763
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HRID 342763 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 3283Diethyl Ether촉매HCID 962Water용매HCID 1004Phosphoric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-217ca2d00562468ea793a75aa79840d8
출처 데이터셋
uspto-grants-1999_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05859051

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