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Sodium Hydroxide → HCID 59700608, 화합물

HRID 902022
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HRID 902022 반응식
Br[C:2]1[C:3]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[N:12]=2)=[N:4][N:5]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=12.[F:18][C:19]1[CH:24]=[CH:23][C:22](B(O)O)=[CH:21][CH:20]=1.[OH-].[Na+]>COCCOC.CCOC(C)=O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[F:18][C:19]1[CH:24]=[CH:23][C:22]([C:2]2[C:3]([C:11]3[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[N:12]=3)=[N:4][N:5]3[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=23)=[CH:21][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 14798Sodium HydroxideHCID 2856454-Fluorophenylboronic acidHCID 59700618HCID 59700618, 화합물

생성물 1

HCID 59700608HCID 59700608, 화합물수율 62%

시약·촉매·용매 3

HCID 178418397HCID 178418397, 화합물촉매
HCID 8071
1,2-Dimethoxyethane
용매
HCID 8857Ethyl Acetate용매

실험 절차

A solution of 3-bromo-2-(6-methyl-pyridin-2-yl)-pyrazolo[1,5-a]pyridine (0.25 g, 0.9 mmol) and p-fluorophenyl-boronic acid (0.15 g, 1.04 mmol), in DME (10 mL) is purged with argon. The solution is treated with NaOH (0.07 g, 1.7 mmol) and (PPh3)4Pd (0.05 g, 0.04 mmol) then heated at reflux overnight. The reaction is then cooled, diluted in EtOAc, and washed with water and brine. The organic solution is dried over MgSO4 and the solvent removed in vacuo. The residue is purified by silica gel column chromatography using a mixture of hexanes/EtOAc to afford 0.164 g (62%) of desired product as a white solid. UV (95% EtOH) λmax 248 nm (ε 20386). TOF MS ES+ exact mass calculated for C19H14FN3 (p+1): m/z=304.1250. Found: 304.1249. Anal. Calcd for C19H14FN3: C, 75.23; H, 4.65; N, 13.85. Found: C, 75.10; H, 4.76; N, 13.70.

후처리

  1. temperaturethen heated
  2. temperatureat reflux overnight
  3. temperatureThe reaction is then cooled
  4. washwashed with water and brine
  5. dry with materialThe organic solution is dried over MgSO4
  6. customthe solvent removed in vacuo
  7. customThe residue is purified by silica gel column chromatography
  8. additiona mixture of hexanes/EtOAc

출처 및 근거

ORD 기록
ord-11040ec29c724c648beed0e196d48992
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07365066B2

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