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Dimethylformamide → Methyl 2-methyl-3-(methylthio)-4-(pentafluoroethyl)benzoate

HRID 41857
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HRID 41857 반응식
F[C:2]1[C:3]([CH3:19])=[C:4]([CH:9]=[CH:10][C:11]=1[C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14])[C:5]([O:7][CH3:8])=[O:6].CN(C)C=O.[CH3:25][S-:26].[Na+]>C(OCC)(=O)C>[CH3:19][C:3]1[C:2]([S:26][CH3:25])=[C:11]([C:12]([F:18])([F:17])[C:13]([F:16])([F:15])[F:14])[CH:10]=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 4378561Sodium methanethiolateHCID 86661429HCID 86661429, 화합물

생성물 1

HCID 86661431Methyl 2-methyl-3-(methylthio)-4-(pentafluoroethyl)benzoate수율 55.5%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

2.1 g (7.34 mmol) of methyl 3-fluoro-2-methyl-4-(pentafluoroethyl)benzoate were introduced into 20 ml of N,N-dimethylformamide and then admixed with 758 mg (95% by weight; 10.3 mmol) of sodium thiomethoxide. The mixture was stirred at RT for 2 hours and then freed from the solvent. The residue was taken up in ethyl acetate and water, the aqueous phase was extracted twice with ethyl acetate, and, finally, the combined organic phases were dried and freed from the solvent. The residue was purified by chromatography, giving 1.28 g of clean product.

후처리

  1. extractionwater, the aqueous phase was extracted twice with ethyl acetate
  2. customfinally, the combined organic phases were dried
  3. customThe residue was purified by chromatography

출처 및 근거

ORD 기록
ord-cf64531ad986452cbe6b030f12fe3a02
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08536097B2

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