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Methanol → HCID 58326407, 화합물

HRID 1666191
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인쇄 미리보기

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HRID 1666191 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[N:12]([C:13]3[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=3[Cl:20])[N:11]=[C:10]([C:21]([OH:23])=[O:22])[CH2:9]2)=[CH:4][CH:3]=1.CO.[CH3:26]C1C=CC(S(O)(=O)=O)=CC=1.O>C1(C)C=CC=CC=1>[CH3:26][O:22][C:21]([C:10]1[CH2:9][CH:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)[N:12]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][C:14]=2[Cl:20])[N:11]=1)=[O:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 521998p-Toluenesulfonic acid monohydrateHCID 11773086HCID 11773086, 화합물

생성물 1

HCID 58326407HCID 58326407, 화합물수율 498.2%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
80 °C

실험 절차

A mixture of 5-(4-chloro-phenyl)-1-(2,4-dichloro-phenyl)-4,5-dihydro-1H-pyrazole-3-carboxylic acid (78.0 g, 0.21 mol), methanol 150 mL, p-TsOH.H2O (0.042 mol) in toluene (350 mL) was stirred for 24 hours at 80° C. The reaction mixture was cooled to room temperature and the solvent was concentrated in vacuo. The residue was taken up in EtOAc (300 mL) and subsequently washed with sat. aq. NH4Cl and water and dried. The solvent was removed in vacuo to yield the title compound (80.27 g, 99%) white solid.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. concentrationthe solvent was concentrated in vacuo
  3. washsubsequently washed with sat. aq. NH4Cl and water
  4. customdried
  5. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-90a23f7868354de8939ed007c3522cf3
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08044053B2

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