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Potassium Hydroxide → HCID 18980957, 화합물

HRID 482618
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HRID 482618 반응식
[F:1][C:2]([F:32])([F:31])[O:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([N:13]2[CH2:17][CH:16]([N:18]([CH3:23])[C:19]([O:21][CH3:22])=[O:20])[C:15]([C:24]3[CH:29]=[CH:28][C:27]([OH:30])=[CH:26][CH:25]=3)=[N:14]2)=[O:12])=[CH:6][CH:5]=1.[OH-].[K+].I[CH2:36][CH2:37][CH3:38]>CS(C)=O.C(OCC)C.O>[F:32][C:2]([F:1])([F:31])[O:3][C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11]([N:13]2[CH2:17][CH:16]([N:18]([CH3:23])[C:19]([O:21][CH3:22])=[O:20])[C:15]([C:24]3[CH:29]=[CH:28][C:27]([O:30][CH2:36][CH2:37][CH3:38])=[CH:26][CH:25]=3)=[N:14]2)=[O:12])=[CH:6][CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 14797Potassium HydroxideHCID 336431-IodopropaneHCID 135703328HCID 135703328, 화합물

생성물 1

HCID 18980957HCID 18980957, 화합물

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매
HCID 3283
Diethyl Ether
용매

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온도
50 °C

실험 절차

To 1.0 g (2.2 mmole) of N-(4-trifluoromethoxyphenyl)-3-(4-hydroxyphenyl)-4-(N-methyl-N-(methoxycarbonyl)amino)-4,5-dihydro-1H-pyrazole-1-carboxamide (Example 297) dissolved in 7.5 ml of dimethylsulfoxide was added 0.35 g (2.8 mmole) of 45% aqueous potassium hydroxide and 1.02 g (6.0 mmole) of 1-iodopropane. The mixture was warmed to 50° C. for 30 minutes and diluted with diethyl ether and water. The organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered, concentrated in vacuo, and chromatographed over silica gel using hexane and diethyl ether to yield the title compound, a white solid, mp 153°-155° C.

후처리

  1. washThe organic layer was washed with brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customchromatographed over silica gel

출처 및 근거

ORD 기록
ord-4eae1f4aa6b74042a2dcaa7fa58a8b4d
출처 데이터셋
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05798311

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