Tetrahydrofuran → HCID 57712427, 화합물

HRID 1983053노트

반응식

HRID 1983053 반응식
[Cl:1][C:2]([Cl:20])([F:19])[S:3][C:4]1[CH:5]=[N:6][N:7]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)[C:8]=1N.O1CCCC1.N(OC(C)(C)C)=O>O>[Cl:20][C:2]([Cl:1])([F:19])[S:3][C:4]1[CH:5]=[N:6][N:7]([CH2:10][C:11]2[CH:12]=[CH:13][C:14]([O:17][CH3:18])=[CH:15][CH:16]=2)[CH:8]=1

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 10906Tert-Butyl nitriteHCID 23149166HCID 23149166, 화합물

생성물 1

HCID 57712427HCID 57712427, 화합물수율 94.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1.04 g of 4-{[dichlorofluoromethyl]thio}-1-(4-methoxybenzyl)-1H-pyrazole-5-amine was dissolved to 20 ml of tetrahydrofuran. 1.55 g of t-butyl nitrite was added to the solution, followed by refluxed for 3 hours. After the reaction mixture was cooled to room temperature, water was added to the reaction mixture, and extracted with diethyl ether. The organic layer was washed with water, dried over sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.94 g of 4-{[dichlorofluoromethyl]thio}-1-(4-methoxybenzyl)-1H-pyrazole.

후처리

  1. temperatureby refluxed for 3 hours
  2. extractionextracted with diethyl ether
  3. washThe organic layer was washed with water
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-efeb9e234444491db013bdb1dea1239b
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07541374B2

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