Water → 1-[3-Chloro-4-(tetrahydro-pyran-4-sulfonyl)-phenyl]-ethanone

HRID 1098755노트

반응식

HRID 1098755 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:15](=[O:17])[CH3:16])[CH:5]=[CH:6][C:7]=1[S:8][CH:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1.[OH:18]OS([O-])=O.[K+].[OH2:24]>CO.O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]([C:15](=[O:17])[CH3:16])[CH:5]=[CH:6][C:7]=1[S:8]([CH:9]1[CH2:10][CH2:11][O:12][CH2:13][CH2:14]1)(=[O:18])=[O:24]

참가 물질

6

반응물 3

HCID 962Water2회HCID 23707502Potassium hydroxy sulfiteHCID 595061481-[3-Chloro-4-(tetrahydro-pyran-4-ylsulfanyl)-phenyl]-ethanone

생성물 1

HCID 595062921-[3-Chloro-4-(tetrahydro-pyran-4-sulfonyl)-phenyl]-ethanone수율 67%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of the product obtained from step 2 (1.38 g, 5.10 mmol) in methanol (25 ml) and tetrahydrofurane (25 ml) was added drop wise to a solution of oxone (5.64 g, 9.17 mmol) in water (25 ml) at 0° C. The suspension was stirred 2 days at RT. Water (25 ml) was added and the reaction mixture was extracted with DCM. The combined organic phases were washed with brine and dried over magnesium sulphate. Evaporation and purification of the crude product by silica gel chromatography using ethyl acetate/n-heptane gave the desired product (1.04 g, 67%).

후처리

  1. extractionthe reaction mixture was extracted with DCM
  2. washThe combined organic phases were washed with brine
  3. dry with materialdried over magnesium sulphate
  4. customEvaporation and purification of the crude product by silica gel chromatography

출처 및 근거

ORD 기록
ord-db988866fb8f49d886201e663ac51506
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143242B2

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