Tetrahydrofuran → HCID 178503597, 화합물

HRID 628542노트

반응식

HRID 628542 반응식
Cl[C:2]1[N:6](C)[N:5]=[C:4]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH:15]([CH3:17])[CH3:16])=[C:10]([CH3:18])[CH:9]=2)[C:3]=1[CH:19]=[O:20].O1CCCC1.[CH3:26][S-:27].[Na+]>O>[CH:19]([C:3]1[C:4]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH:15]([CH3:17])[CH3:16])=[C:10]([CH3:18])[CH:9]=2)=[N:5][NH:6][C:2]=1[S:27][CH3:26])=[O:20]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 4378561Sodium methanethiolateHCID 118001333HCID 118001333, 화합물

생성물 1

HCID 178503597HCID 178503597, 화합물수율 104.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

At room temperature, to a mixture of 5-chloro-4-formyl-3-(4-isopropoxy-3-methyl-phenyl)-1-methyl-1H-pyrazole (described in Reference Preparation example 96) 10 g and tetrahydrofuran 100 ml was added sodium thiomethoxide 2.9 g and the resulting mixture was stirred for eight hours. To the reaction mixture was added water 50 mL and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with water and was dried over anhydrous magnesium sulfate, and was then concentrated under reduced pressure. The resulting residue was subjected to a silica gel column chromatography to give 4-formyl-3-(4-isopropoxy-3-methyl-phenyl)-5-methylthio-1H-pyrazole 10.4 g.

후처리

  1. extractionthe resulting mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialwas dried over anhydrous magnesium sulfate
  4. concentrationwas then concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-624def0aa5e24af98dda894305079b14
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09314023B2

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