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1-(2-Amino-1,3-thiazol-5-yl)cyclobutan-1-ol → 5-Cyclobutyl-1,3-thiazol-2-amine

HRID 2085489
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HRID 2085489 반응식
[NH2:1][C:2]1[S:3][C:4]([C:7]2(O)[CH2:10][CH2:9][CH2:8]2)=[CH:5][N:6]=1>FC(F)(F)C(O)=O.[OH-].[OH-].[Pd+2]>[CH:7]1([C:4]2[S:3][C:2]([NH2:1])=[N:6][CH:5]=2)[CH2:10][CH2:9][CH2:8]1
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참가 물질

4

반응물 1

HCID 227313761-(2-Amino-1,3-thiazol-5-yl)cyclobutan-1-ol

생성물 1

HCID 129914235-Cyclobutyl-1,3-thiazol-2-amine수율 79%

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of 1-(2-amino-thiazol-5-yl)cyclobutanol (Preparation 1; 6.6 g, 39 mmol) in trifluoroacetic acid (150 mL) was treated with 20% palladium hydroxide on carbon (2.3 g). The mixture was evacuated and purged with nitrogen (3 times), then was evacuated and purged with hydrogen gas (50 psi). The mixture was shaken for 24 hours and was evacuated and purged with nitrogen. The mixture was then filtered through Celite which was rinsed with methanol. The organic solvent was removed in vacuo, ethylacetate was added, followed by 29% ammonium hydroxide solution. The aqueous and organic layers were separated and the aqueous layer was extracted with ethylacetate. The combined organic layers were washed with brine, were dried (MgSO4), were filtered, and the solvent was removed in vacuo. The resulting residue was purified by silica gel chromatography (40:1:1 CHCl3—MeOH—NH4OH) to afford 4.75 g of 5-cyclobutyl-thiazol-2-ylamine, the title compound. 1HNMR (400 MHz, DMSO-d6): 6.66(s,2H), 6.57(s, 2H), 3.43 (m,1H), 2.20 (m,2H), 1.98-1.7 (m,4H).

후처리

  1. customThe mixture was evacuated
  2. custompurged with nitrogen (3 times)
  3. customwas evacuated
  4. custompurged with hydrogen gas (50 psi)
  5. customwas evacuated
  6. custompurged with nitrogen
  7. filtrationThe mixture was then filtered through Celite which
  8. washwas rinsed with methanol
  9. customThe organic solvent was removed in vacuo, ethylacetate
  10. additionwas added
  11. customThe aqueous and organic layers were separated
  12. extractionthe aqueous layer was extracted with ethylacetate
  13. washThe combined organic layers were washed with brine
  14. dry with materialwere dried (MgSO4)
  15. filtrationwere filtered
  16. customthe solvent was removed in vacuo
  17. customThe resulting residue was purified by silica gel chromatography (40:1:1 CHCl3—MeOH—NH4OH)

출처 및 근거

ORD 기록
ord-1943e7c6151e4f8cb49a5227acd7e5d0
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06720427B2

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