2,6-Dibromopyridine → 2-{3-[3,5-Bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}-6-bromopyridine

HRID 2206901

반응식

HRID 2206901 반응식
[F:1][C:2]([F:23])([F:22])[C:3]1[CH:4]=[C:5]([C:13]2([C:18]([F:21])([F:20])[F:19])[CH2:17][CH2:16][NH:15][CH2:14]2)[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[Br:24][C:25]1[CH:30]=[CH:29][CH:28]=[C:27](Br)[N:26]=1.C(N(CC)C(C)C)(C)C.CC(N(C)C)=O>C(OCC)(=O)C>[F:12][C:9]([F:10])([F:11])[C:7]1[CH:6]=[C:5]([C:13]2([C:18]([F:21])([F:19])[F:20])[CH2:17][CH2:16][N:15]([C:27]3[CH:28]=[CH:29][CH:30]=[C:25]([Br:24])[N:26]=3)[CH2:14]2)[CH:4]=[C:3]([C:2]([F:22])([F:1])[F:23])[CH:8]=1

참가 물질

6

반응물 4

HCID 122742,6-DibromopyridineHCID 31374DimethylacetamideHCID 81531DiisopropylethylamineHCID 532621863-[3,5-Bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidine

생성물 1

HCID 871585732-{3-[3,5-Bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}-6-bromopyridine수율 92.3%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 3-[3,5-bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidine (3.0 g), 2,6-dibromopyridine (2.22 g), N,N-diisopropylethylamine (2.2 g) and dimethylacetamide (15 ml) was reacted at 160° C. in a sealed tube for 1 hour. Upon the completion of the reaction, the mixture was added with ethyl acetate, washed with water and then saturated brine, dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography to obtain 2-{3-[3,5-bis(trifluoromethyl)phenyl]-3-(trifluoromethyl)pyrrolidin-1-yl}-6-bromopyridine (4.0 g).

후처리

  1. customwas reacted at 160° C. in a sealed tube for 1 hour
  2. customUpon the completion of the reaction
  3. washwashed with water
  4. dry with materialsaturated brine, dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-2b8d32244fdf469d902e787cde430c9e
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09375000B2

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