Triethylamine → Methyl-phenyl-carbamic Acid 3-chloro-5-trifluoromethyl-pyridin-2-yl Ester

HRID 1179866

반응식

HRID 1179866 반응식
[Cl:1][C:2]1[C:3]([OH:12])=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.[I-].C[N+]1C=CN([C:20](=[O:29])[N:21]([CH3:28])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)C=1.C(N(CC)CC)C>C(#N)C>[Cl:1][C:2]1[C:3]([O:12][C:20](=[O:29])[N:21]([CH3:28])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[N:4][CH:5]=[C:6]([C:8]([F:11])([F:9])[F:10])[CH:7]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 7254363-Chloro-5-(trifluoromethyl)pyridin-2-olHCID 109478841-methyl-3-(methyl-phenyl-carbamoyl)-3H-imidazol-1-ium iodide

생성물 1

HCID 69518742Methyl-phenyl-carbamic Acid 3-chloro-5-trifluoromethyl-pyridin-2-yl Ester수율 15%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A solution of 3-chloro-5-(trifluoromethyl)-2-pyridinol (0.59 g, 3.00 mmol), 1-methyl-3-(methyl -phenyl-carbamoyl)-3H-imidazol-1-ium iodide (1.03 g, 3.00 mmol) and triethylamine (0.42 ml, 3.00 mmol) in acetonitrile (15 ml) was stirred at room temperature for 18 hours. The solvent was evaporated in vacuo and the residue was purified by flash column chromatography (SiO2, ethyl acetate:heptane (15:85)) yielding the title compound (146 mg, 15% yield) as a white solid.

후처리

  1. customThe solvent was evaporated in vacuo
  2. customthe residue was purified by flash column chromatography (SiO2, ethyl acetate:heptane (15:85))

출처 및 근거

ORD 기록
ord-8967cdf36b564778a0f0050d41f96201
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07279470B2

연결된 노트

불러오는 중…