Methyl vinyl sulfone → 5-methyl-1-((1-(2-(methylsulfonyl)ethoxy)cyclooctyl)methyl)-1H-pyrazole

HRID 588690노트

반응식

HRID 588690 반응식
[H-].[Na+].[CH3:3][C:4]1[N:8]([CH2:9][C:10]2([OH:18])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[N:7]=[CH:6][CH:5]=1.[CH:19]([S:21]([CH3:24])(=[O:23])=[O:22])=[CH2:20].[NH4+].[Cl-]>O1CCCC1>[CH3:3][C:4]1[N:8]([CH2:9][C:10]2([O:18][CH2:20][CH2:19][S:21]([CH3:24])(=[O:23])=[O:22])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17]2)[N:7]=[CH:6][CH:5]=1

참가 물질

6

반응물 4

HCID 19354Methyl vinyl sulfoneHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 866812711-((5-methyl-1H-pyrazol-1-yl)methyl)cyclooctanol

생성물 1

HCID 894992895-methyl-1-((1-(2-(methylsulfonyl)ethoxy)cyclooctyl)methyl)-1H-pyrazole

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Sodium hydride (60% dispersion in mineral oil, 200 mg) was added to a stirred solution of EXAMPLE 65A (667 mg) in tetrahydrofuran (10 mL) and the mixture was stirred at room temperature for 30 minutes before the addition of methyl vinyl sulfone (1.27 g). The mixture was stirred at room temperature for 3 hours. Aqueous NH4Cl was added to quench the reaction and the mixture was extracted with ethyl acetate (three times) and the combined organic layers were washed with water and brine, dried over Na2SO4, and filtered. The filtrate was concentrated to provide the crude product.

후처리

  1. customto quench
  2. customthe reaction
  3. extractionthe mixture was extracted with ethyl acetate (three times)
  4. washthe combined organic layers were washed with water and brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-d65e717c32894ff2b4f6671069e1450c
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09227963B2

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