Bromine → 1-(4-Pentylphenyl)-2-(2,6-difluoropyridine-3-yl)acetylene

HRID 1591024

반응식

HRID 1591024 반응식
Br[C:2]1[C:3]([F:9])=[N:4][C:5]([F:8])=[CH:6][CH:7]=1.F[C:11]1[CH:16]=[CH:15][CH:14]=[C:13](F)N=1.C([N-][CH:22]([CH3:24])[CH3:23])(C)C.[Li+].BrBr>Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH2:13]([C:7]1[CH:6]=[CH:5][C:24]([C:22]#[C:23][C:2]2[C:3]([F:9])=[N:4][C:5]([F:8])=[CH:6][CH:7]=2)=[CH:3][CH:2]=1)[CH2:14][CH2:15][CH2:16][CH3:11]

참가 물질

6

반응물 4

HCID 24408BromineHCID 739342,6-DifluoropyridineHCID 2724682Lithium diisopropylamideHCID 197657393-Bromo-2,6-difluoropyridine

생성물 1

HCID 197657611-(4-Pentylphenyl)-2-(2,6-difluoropyridine-3-yl)acetylene

시약·촉매·용매 1

HCID 178418476HCID 178418476, 화합물촉매

실험 절차

0,2 mM of Pd(Ph3P)2Cl2 and 0,1 mM of CuJ are added to a mixture of 0,01 M of 3-bromo-2,6-difluoropyridine (preparation: 2,6-difluoropyridine is reacted with lithiumdiisopropylamide (LDA) as described in example 3a, then Br2 is added at -60° to -70°. The mixture is allowed to warm up to room temperature and worked up, the product is purified by distillation), 0,01 M of 4-pentylphenylacetylene and 200 ml of triethylamine. The mixture is stirred for 8 hours at room temperature; after customary work-up and purification by crystallization and chromatography 1-(4-pentylphenyl)-2-(2,6-difluoropyridine-3-yl)acetylene is obtained.

후처리

  1. custompreparation
  2. distillationthe product is purified by distillation), 0,01 M of 4-pentylphenylacetylene and 200 ml of triethylamine
  3. customafter customary work-up and purification
  4. customby crystallization

출처 및 근거

ORD 기록
ord-985d2f9b05bf4439be574206950131d3
출처 데이터셋
uspto-grants-1993_04
특허 번호
US05205962

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