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2,5-Difluorobenzohydrazide → Toluene-4-sulfonic acid 3-tert-butyl-7-(2,5-difluorophenyl)-4-methylpyrazolo[1,5-d][1,2,4]triazin-2-yl ester

HRID 985432
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인쇄 미리보기

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HRID 985432 반응식
[C:1]([C:4]1[NH:8][N:7]=[C:6]([O:9][S:10]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=2)(=[O:12])=[O:11])[C:5]=1[C:20]([CH3:23])([CH3:22])[CH3:21])(=O)[CH3:2].[F:24][C:25]1[CH:34]=[CH:33][C:32]([F:35])=[CH:31][C:26]=1[C:27]([NH:29][NH2:30])=O>C1(C)C(C)=CC=CC=1>[C:20]([C:5]1[C:6]([O:9][S:10]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=2)(=[O:12])=[O:11])=[N:7][N:8]2[C:4]=1[C:1]([CH3:2])=[N:30][N:29]=[C:27]2[C:26]1[CH:31]=[C:32]([F:35])[CH:33]=[CH:34][C:25]=1[F:24])([CH3:23])([CH3:22])[CH3:21]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 27740742,5-DifluorobenzohydrazideHCID 225068935-Acetyl-4-tert-butyl-3-(4-methylphenyl)sulfonyloxypyrazole

생성물 1

HCID 86587510Toluene-4-sulfonic acid 3-tert-butyl-7-(2,5-difluorophenyl)-4-methylpyrazolo[1,5-d][1,2,4]triazin-2-yl ester수율 53.4%

시약·촉매·용매 1

HCID 7237O-Xylene용매

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온도
180 °C

실험 절차

5-Acetyl-4-tert-butyl-3-(4-methylphenyl)sulfonyloxypyrazole (0.4 g, 1.19 mmol) was dissolved in xylene (20 ml) with 2,5-difluorobenzoic hydrazide (0.225 g, 1.31 mmol) and heated under reflux for 14 h. The xylene was removed by evaporation and replaced with Dowtherm A (15 ml) and heated at 180° C. for 4 h. The reaction mixture was allowed to cool to room temperature and poured directly onto a silica column and eluted with dichloromethane then 1-5% ethyl acetate/dichloromethane to give the required product (0.3 g) as a white solid. 1H NMR (360 MHz, CDCl3) δ 1.64 (9H, s), 2.42 (3H, s), 3.11 (3H, s), 7.11-7.83 (8H, m); MS (ES+) m/e 473 [MH]+.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 14 h
  3. customThe xylene was removed by evaporation
  4. temperatureto cool to room temperature
  5. additionpoured directly onto a silica column
  6. washeluted with dichloromethane

출처 및 근거

ORD 기록
ord-77d026fe82574db490cad0b02f5a2128
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06872720B2

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