Tetrahydrofuran → HCID 57712427、化合物

HRID 1983053ノート

反応式

HRID 1983053 の反応式
[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

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 10906Tert-Butyl nitriteHCID 23149166HCID 23149166、化合物

生成物 1

HCID 57712427HCID 57712427、化合物収率 94.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-efeb9e234444491db013bdb1dea1239b
出典データセット
uspto-grants-2009_06
特許番号
US07541374B2

反応ノート

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