3,4-dihydro-2H-pyran → 2-(5-Bromopentyloxy)tetrahydro-2H-pyran

HRID 223671

반응식

HRID 223671 반응식
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][OH:7].[O:8]1[CH:13]=[CH:12][CH2:11][CH2:10][CH2:9]1>P(Cl)(Cl)(Cl)=O.C(OCC)C>[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][CH:9]1[CH2:10][CH2:11][CH2:12][CH2:13][O:8]1

참가 물질

5

반응물 2

HCID 80803,4-dihydro-2H-pyranHCID 1187091-Pentanol, 5-bromo-

생성물 1

HCID 27869332-(5-Bromopentyloxy)tetrahydro-2H-pyran

시약·촉매·용매 2

HCID 24813Phosphorus oxychloride촉매HCID 3283Diethyl Ether용매

실험 절차

To 36 g of 5-bromopentan-1-ol were added 24.72 ml of 2,3-dihydropyran and 3 drops of phosphorus oxychloride under cooling in an ice bath, and the mixture was stirred overnight at room temperature. The reaction mixture was diluted with diethyl ether, washed with 5% aqueous potassium hydroxide, water, a saturated aqueous solution of sodium chloride, dried over magnesium sulphate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using a mixture of ethyl acetate and hexane (1:19) as eluent to give 49.5 g of the subtitle compound having the following physical characteristics:

후처리

  1. temperatureunder cooling in an ice bath
  2. washwashed with 5% aqueous potassium hydroxide, water
  3. dry with materiala saturated aqueous solution of sodium chloride, dried over magnesium sulphate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel using
  6. additiona mixture of ethyl acetate and hexane (1:19) as eluent

출처 및 근거

ORD 기록
ord-963694e4650e47aba6e53ac71fff74c3
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04355170

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