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5-Bromo-4-methyl-1,3-thiazole → 7-(1-Ethyl-propyl)-2,5-dimethyl-3-(4-methyl-thiazol-5-yl)-pyrazolo[1,5-a]pyrimidine

HRID 1660741
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HRID 1660741 반응식
Br[C:2]1[S:6][CH:5]=[N:4][C:3]=1[CH3:7].[CH2:8]([CH:10]([C:13]1[N:18]2[N:19]=[C:20]([CH3:23])[C:21](I)=[C:17]2[N:16]=[C:15]([CH3:24])[CH:14]=1)[CH2:11][CH3:12])[CH3:9]>O1CCCC1.[Zn].Cl[Pd]Cl.C1(P(C2C=CC=CC=2)[C-]2C=CC=C2)C=CC=CC=1.[C-]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=C1.[Fe+2]>[CH2:8]([CH:10]([C:13]1[N:18]2[N:19]=[C:20]([CH3:23])[C:21]([C:2]3[S:6][CH:5]=[N:4][C:3]=3[CH3:7])=[C:17]2[N:16]=[C:15]([CH3:24])[CH:14]=1)[CH2:11][CH3:12])[CH3:9]
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참가 물질

6

반응물 2

HCID 150209975-Bromo-4-methyl-1,3-thiazoleHCID 248985233-Iodo-2,5-dimethyl-7-(pentan-3-yl)pyrazolo[1,5-a]pyrimidine

생성물 1

HCID 674287127-(1-Ethyl-propyl)-2,5-dimethyl-3-(4-methyl-thiazol-5-yl)-pyrazolo[1,5-a]pyrimidine수율 79.1%

시약·촉매·용매 3

HCID 23994Zinc촉매2회
HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 8028Tetrahydrofuran용매

실험 절차

Add Rieke® zinc (10 g in 100 mL of THF, 13.2 mL, 18.48 mmol) to 5-bromo-4-methylthiazole (2.13 g, 18.48 mmol) and heat at reflux for 2 h. Cool the mixture to room temperature and settle the zinc down by centrifuge. Bubble nitrogen gas through 7-(1-ethyl-propyl)-3-iodo-2,5-dimethyl-pyrazolo[1,5-a]pyrimidine (900 mg, 2.62 mmol) in dry tetrahydrofuran (10 mL) and add the organozinc bromide solution followed by addition of [1,1′-bis(diphenylphosphino)ferrocene]-dichloropalladium(II) (106 mg, 0.13 mmol). Stir the reaction mixture under reflux overnight and cool to room temperature. Add ammonium chloride solution to the reaction mixture and extract with dichloromethane. Dry the organic portion over sodium sulfate, filter, and remove the solvent under vacuum. Purify the crude product by silica gel column chromatography, elueting with hexane/ethyl acetate (3/1) to obtain the title compound (652 mg, 79%). 1H NMR (400 MHz, CDCl3): δ 8.80 (s, 1H), 6.48 (s, 1H), 3.63 (m, 1H), 2.57 (s, 3H), 2.43 (s, 3H), 2.40 (s, 3H), 1.85 (m, 4H), 0.90 (t, 6H, J=7.3Hz). ES/MS m/z 315 (M+1)+.

후처리

  1. temperatureheat
  2. temperatureat reflux for 2 h
  3. temperatureunder reflux overnight
  4. temperaturecool to room temperature
  5. extractionAdd ammonium chloride solution to the reaction mixture and extract with dichloromethane
  6. dry with materialDry the organic portion over sodium sulfate
  7. filtrationfilter
  8. customremove the solvent under vacuum
  9. customPurify the crude product by silica gel column chromatography

출처 및 근거

ORD 기록
ord-718a48d476884e51a2b7c3b89c1b7d8c
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030304B2

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