p-Toluenesulfonic acid monohydrate → 2-(2-(4-bromo-2-(trifluoromethyl)phenoxy)ethoxy)tetrahydro-2H-pyran

HRID 912511노트

반응식

HRID 912511 반응식
[Br:1][C:2]1[CH:11]=[CH:10][C:5]([O:6][CH2:7][CH2:8][OH:9])=[C:4]([C:12]([F:15])([F:14])[F:13])[CH:3]=1.[OH2:16].[C:17]1(C)C=[CH:21][C:20](S(O)(=O)=O)=[CH:19][CH:18]=1>C1COCC1.C(=O)(O)[O-].[Na+]>[Br:1][C:2]1[CH:11]=[CH:10][C:5]([O:6][CH2:7][CH2:8][O:9][CH:21]2[CH2:20][CH2:19][CH2:18][CH2:17][O:16]2)=[C:4]([C:12]([F:13])([F:14])[F:15])[CH:3]=1

참가 물질

5

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 576575832-(4-Bromo-2-(trifluoromethyl)phenoxy)-ethanol

생성물 1

HCID 576575782-(2-(4-bromo-2-(trifluoromethyl)phenoxy)ethoxy)tetrahydro-2H-pyran수율 2,164%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 516892Sodium Bicarbonate용매

실험 절차

A mixture of 2-(4-bromo-2-(trifluoromethyl)phenoxy)ethanol (16 g), 3,4-dihydro-2H-puran (9.5 g) and p-toluenesulfonic acid hydrate (0.5 g) in THF (100 ml) was stirred at room temperature for 1 hour then diluted with 5% sodium bicarbonate (300 ml) and extracted with ethyl acetate (500 ml). Organic layer was then dried over sodium sulphate, solvent removed under vacuum to give expected product (21 g).

후처리

  1. extractionextracted with ethyl acetate (500 ml)
  2. dry with materialOrganic layer was then dried over sodium sulphate, solvent
  3. customremoved under vacuum

출처 및 근거

ORD 기록
ord-35316238b9c6450ea84fb7cf893a78e4
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026236B2

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