2,2,2-Trifluoroacetophenone → HCID 178498430, 화합물

HRID 60128

반응식

HRID 60128 반응식
S(Cl)(Cl)=O.[F:5][C:6]([F:16])([F:15])[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=O.[CH3:17][O:18][C:19]([C:21]1[CH:26]=[CH:25][N:24]=[C:23]([NH2:27])[CH:22]=1)=[O:20].[OH-].[Na+]>N1C=CC=CC=1>[F:5][C:6]([F:16])([F:15])/[C:7](=[N:27]\[C:23]1[CH:22]=[C:21]([CH:26]=[CH:25][N:24]=1)[C:19]([O:18][CH3:17])=[O:20])/[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

참가 물질

6

반응물 4

HCID 99052,2,2-TrifluoroacetophenoneHCID 14798Sodium HydroxideHCID 24386Thionyl ChlorideHCID 236984Methyl 2-aminopyridine-4-carboxylate

생성물 1

HCID 178498430HCID 178498430, 화합물수율 27.7%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Thionyl chloride (2.2 ml) was added at 0° C. to a pyridine (4.8 ml) solution of 2,2,2-trifluoro-1-phenylethanone (5.1 g) and 2-aminopyridine-4-carboxylic acid methyl ester (4.5 g). The temperature of the reaction solution was increased to room temperature, and the reaction solution was then stirred for 1 hour. Thereafter, the reaction solution was poured into a 1 N sodium hydroxide aqueous solution, and the mixed solution was then extracted with ethyl acetate. Organic layers were gathered, and the gathered organic layer was then dried over anhydrous sodium sulfate. After that, the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel column chromatography (silica gel: eluent; heptane:ethyl acetate=2:1-1:1), so as to obtain the title compound (2.5 g) in the form of a yellow liquid.

후처리

  1. extractionthe mixed solution was then extracted with ethyl acetate
  2. dry with materialthe gathered organic layer was then dried over anhydrous sodium sulfate
  3. distillationAfter that, the solvent was distilled away under reduced pressure
  4. customThe obtained residue was purified by silica gel column chromatography (silica gel: eluent; heptane:ethyl acetate=2:1-1:1)

출처 및 근거

ORD 기록
ord-7b51dea22de641019236184e5be34a55
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440970B2

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