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2,3-Dibromobutane → HCID 59632583, 화합물

HRID 2369051
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HRID 2369051 반응식
[Mg].Br[CH:3]([CH3:7])[CH:4](Br)[CH3:5].C[O:9][C:10]([C:12]1[CH:16]=[C:15]([C:17]2[S:18][C:19]([C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([S:28]([CH3:31])(=[O:30])=[O:29])[CH:23]=3)=[CH:20][CH:21]=2)[N:14]([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=2[Cl:38])[N:13]=1)=O.[NH4+].[Cl-]>C1COCC1>[Cl:38][C:33]1[CH:34]=[CH:35][CH:36]=[CH:37][C:32]=1[N:14]1[C:15]([C:17]2[S:18][C:19]([C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([S:28]([CH3:31])(=[O:30])=[O:29])[CH:23]=3)=[CH:20][CH:21]=2)=[CH:16][C:12]([C:10]2([OH:9])[CH2:5][CH2:4][CH2:3][CH2:7]2)=[N:13]1
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참가 물질

6

반응물 4

HCID 215082,3-DibromobutaneHCID 25517Ammonium ChlorideHCID 5462224Magnesium2회HCID 59631939HCID 59631939, 화합물

생성물 1

HCID 59632583HCID 59632583, 화합물수율 56.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매
2회

실험 절차

Magnesium turnings (300 mg, 12.5 mmol) was introduced into a oven-dried flask under N2, covered with anhydrous THF (150 mL), and a solution of dibromobutane (0.72 mL, 6.08 mmol) in anhydrous THF (20 mL) was added dropwise at ambient temperature at such a rate that the temperature of the reaction mixture did not rise above 40° C. The mixture was stirred at ambient temperature for 1 h, and the magnesium turnings disappeared. 1-(2-chloro-phenyl)-5-[5-(3-methanesulfonyl-phenyl)thiophen-2-yl]-1H-pyrazole-3-carboxylic acid methyl ester (2.37 g, 5 mmol) was added as a solid, and the resulting dark-purple solution was stirred at room temperature under N2 for 1 h, At 0° C. aqueous NH4Cl solution was added, and then extracted with EtOAc, The combined extracts were washed with brine, dried over Na2SO4. and evaporated in vacuo. The crude product was purified by flash chromatography (0-60% EtOc/hexanes) to afford the title compound as a white solid (1.4 g, 56%). 1HNMR (CDCl3): δ 8.04 (d, 1H), 7.83-7.81 (m, 1H), 7.74-7.71 (m, 1H), 7.57-7.52 (m, 3H), 7.48-7.44 (m, 2H), 7.20 (d, 1H), 6.74 (d, 1H), 6.63 (s, 1H), 3.07 (s, 3H), 2.42 (brs, 1H), 2.20-1.83 (m, 8H). MS(ES) 499 [M+H]+, 481 (M-OH).

후처리

  1. customdid not rise above 40° C
  2. additionwas added
  3. extractionextracted with EtOAc
  4. washThe combined extracts were washed with brine
  5. dry with materialdried over Na2SO4
  6. customand evaporated in vacuo
  7. customThe crude product was purified by flash chromatography (0-60% EtOc/hexanes)

출처 및 근거

ORD 기록
ord-98685b03ab214ee59373495063fce9b7
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703805B2

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