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

HRID 127800

반응식

HRID 127800 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-a7b12ef579b64c6491bfc0e7afa3bd18
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256757

연결된 노트

불러오는 중…