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Diethyl Ether → 4-Trimethylsilyl-2,3,5,6-tetrafluorobenzyl alcohol

HRID 34609
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HRID 34609 반응식
[CH3:1][Si:2]([CH3:22])([CH3:21])[C:3]1[C:16]([F:17])=[C:15]([F:18])[C:6]([CH2:7][O:8]C2CCCCO2)=[C:5]([F:19])[C:4]=1[F:20].C(OCC)(=O)C.C(OCC)C>CO.Cl>[CH3:1][Si:2]([CH3:22])([CH3:21])[C:3]1[C:16]([F:17])=[C:15]([F:18])[C:6]([CH2:7][OH:8])=[C:5]([F:19])[C:4]=1[F:20]
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참가 물질

6

반응물 3

HCID 3283Diethyl EtherHCID 8857Ethyl AcetateHCID 139114812-[4-Trimethylsilyl-2,3,5,6-tetrafluorobenzyloxy]-tetrahydropyran

생성물 1

HCID 139114824-Trimethylsilyl-2,3,5,6-tetrafluorobenzyl alcohol

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매HCID 887Methanol용매

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온도
25 °C

실험 절차

The crude tetrahydropyranyl ether prepared in Stage (i) was dissolved in methanol (20 cm3), and to the stirred solution was added concentrated hydrochloric acid (3 drops). After stirring for 16 hours at the ambient temperature (ca. 25° C.), the reaction mixture was poured into ethyl acetate, washed with water and brine, and dried. Evaporation of the solvent under reduced pressure gave a yellow oil which was subjected to column chromatography on silica gel using petroleum ether (boiling range 40°-60° C.) containing diethyl ether (10% gradually increased to 40% by volume) as eluent to give 4-trimethylsilyl-2,3,5,6-tetrafluorobenzyl alcohol (0.79 g).

후처리

  1. washwashed with water and brine
  2. customdried
  3. customEvaporation of the solvent under reduced pressure
  4. customgave a yellow oil which
  5. temperaturegradually increased to 40% by volume) as eluent

출처 및 근거

ORD 기록
ord-c63bc3ba6643468999e4739e9fb348d1
출처 데이터셋
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04762835

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