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Sodium Hydroxide → HCID 22228131, 화합물

HRID 1744588
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HRID 1744588 반응식
C([CH:3]([C:38]([OH:40])=[O:39])[N:4]([C:19]([C:21]1[C:22]([CH3:37])=[N:23][N:24]([C:26]2[CH:31]=[C:30]([C:32]([F:35])([F:34])[F:33])[CH:29]=[CH:28][C:27]=2[Cl:36])[CH:25]=1)=[O:20])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[C:7]([C:17]#[N:18])[CH:6]=1)C.[OH-].[Na+]>C(O)C>[Cl:36][C:27]1[CH:28]=[CH:29][C:30]([C:32]([F:34])([F:35])[F:33])=[CH:31][C:26]=1[N:24]1[CH:25]=[C:21]([C:19]([N:4]([C:5]2[CH:10]=[CH:9][C:8]([O:11][CH2:12][C:13]([CH3:15])([CH3:16])[CH3:14])=[C:7]([C:17]#[N:18])[CH:6]=2)[CH2:3][C:38]([OH:40])=[O:39])=[O:20])[C:22]([CH3:37])=[N:23]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22227948HCID 22227948, 화합물

생성물 1

HCID 22228131HCID 22228131, 화합물수율 70.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethyl N-[1-(2-Chloro-5-trifluoromethylphenyl)-3-methylpyrazol-4-ylcarbonyl]-N-(3-cyano-4-neopentyloxyphenyl)glycine (1.8 g) was added to ethanol (15 ml). 10% aqueous sodium hydroxide solution (15 ml) was added and the mixture was stirred at a refluxing temperature for 30 min. The solvent was evaporated under reduced pressure, and dilute hydrochloric acid was added. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. A mixed solvent of chloroform-n-hexane was added to the residue to allow crystallization. The crystals were recrystallized from a mixed solvent of diisopropyl ether-n-hexane to give the title compound (1.2 g), melting point: 189–190° C.

후처리

  1. customThe solvent was evaporated under reduced pressure, and dilute hydrochloric acid
  2. additionwas added
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customafter which the solvent was evaporated under reduced pressure
  7. additionA mixed solvent of chloroform-n-hexane was added to the residue
  8. customcrystallization
  9. customThe crystals were recrystallized from a mixed solvent of diisopropyl ether-n-hexane

출처 및 근거

ORD 기록
ord-82c5955f96514239927929bd123c00aa
출처 데이터셋
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07015218B1

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