3,4-dihydro-2H-pyran → 2-[(6-bromohexyl)oxy]tetrahydro-2H-pyran

HRID 228142

반응식

HRID 228142 반응식
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][OH:8].[O:9]1[CH:14]=[CH:13][CH2:12][CH2:11][CH2:10]1>>[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][O:8][CH:10]1[CH2:11][CH2:12][CH2:13][CH2:14][O:9]1

참가 물질

3

반응물 2

HCID 80803,4-dihydro-2H-pyranHCID 779706-Bromo-1-hexanol

생성물 1

HCID 1038602-[(6-bromohexyl)oxy]tetrahydro-2H-pyran수율 91.1%

실험 절차

6-bromo-1-(tetrahydropyranyloxy)hexane was synthesized in the same manner as in Example 1 (the formula (26): step 1). First, 197.8 g (1.09 mol) of 6-bromo-1-hexanol were fed into a 500 mL reactor vessel and cooled to 5° C. or less, and then 102.1 g (1.21 mol) of dihydropyran were dripped at 10° C. or less. After completion of dripping, the mixture was warmed to room temperature and stirred for one hour. The obtained residues were subjected to silica gel column and purified using a mixed solvent of hexane/diisopropylether (IPE) (volume ratio 5:1) as an eluting solvent, and thus 263.4 g of 6-bromo-1-(tetrahydropyranyloxy)hexane were obtained. The yield in this case was 90.9%.

후처리

  1. temperaturecooled to 5° C. or less
  2. customwere dripped at 10° C. or less
  3. custompurified

출처 및 근거

ORD 기록
ord-b00c6b0673e34209909a03f73c6ad8ac
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560731B2

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