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2-Propanone, 1-(acetyloxy)-3-chloro- → Diethyl [(2,3,4-trifluoroanilino)(3-acetoxy-2-oxopropylthio)methylene]malonate

HRID 1382740
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HRID 1382740 반응식
[Na].[F:2][C:3]1[C:22]([F:23])=[C:21]([F:24])[CH:20]=[CH:19][C:4]=1[NH:5][C:6](=[C:8]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[SH:7].[C:25]([O:28][CH2:29][C:30]([CH2:32]Cl)=[O:31])(=[O:27])[CH3:26]>CN(C)C=O>[F:2][C:3]1[C:22]([F:23])=[C:21]([F:24])[CH:20]=[CH:19][C:4]=1[NH:5][C:6](=[C:8]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[S:7][CH2:32][C:30](=[O:31])[CH2:29][O:28][C:25](=[O:27])[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 384132-Propanone, 1-(acetyloxy)-3-chloro-HCID 178472269HCID 178472269, 화합물

생성물 1

HCID 14390992Diethyl [(2,3,4-trifluoroanilino)(3-acetoxy-2-oxopropylthio)methylene]malonate수율 91%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Diethyl [(2,3,4-trifluoroanilino)(mercapto)methylene]malonate sodium salt (5.3 g) was dissolved in N,N-dimethylformamide (70 ml) and thereo 1-acetoxy-3-chloroacetone (2.2 g) was added and the mixture was stirred at room temperature for 30 minutes. The reaction mixture was filtered to remove insoluble materials. After the filtrate was evaporated to dryness under reduced pressure, water was added to the residue and the mixture was extracted with chloroform. The extract was washed with a NaCl solution and dried over anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure to give the title compound (6.0 g) as pale yellow oil.

후처리

  1. filtrationThe reaction mixture was filtered
  2. customto remove insoluble materials
  3. customAfter the filtrate was evaporated to dryness under reduced pressure, water
  4. additionwas added to the residue
  5. extractionthe mixture was extracted with chloroform
  6. washThe extract was washed with a NaCl solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationby distilling off the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-79e335fdd4f24cf792a38d53a3cdc60c
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04808584

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