Ethyl Acetate → HCID 58994234, 화합물

HRID 12664노트

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HRID 12664 반응식
[OH:1][CH2:2][CH2:3][CH2:4][N:5]1[CH:10]=[C:9]([C:11]2[S:12][CH:13]=[CH:14][C:15]=2[CH3:16])[C:8](=[O:17])[NH:7][C:6]1=[O:18].CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O.C(OCC)(=O)C>C1COCC1>[CH3:16][C:15]1[CH:14]=[CH:13][S:12][C:11]=1[C:9]1[C:8](=[O:17])[NH:7][C:6](=[O:18])[N:5]([CH2:4][CH2:3][CH:2]=[O:1])[CH:10]=1

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 159087TriacetoxyperiodinaneHCID 589941881-(3-Hydroxypropyl)-5-(3-methylthiophen-2-yl)pyrimidine-2,4(1H,3H)-dione

생성물 1

HCID 58994234HCID 58994234, 화합물수율 50%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

1-(3-Hydroxy-propyl)-5-(3-methyl-thiophen-2-yl)-1H-pyrimidine-2,4-dione (Prep 28.36 mg, 0.13 mmol) was dissolved in dry THF (5 mL), the solution was cooled to 0° C. and then Dess-Martin periodinane (97 mg, 0.22 mmol) was added under nitrogen. The mixture was stirred at room temperature for 1.5 hours. Ethyl acetate was added and the solution was washed with aqueous saturated NaHCO3 solution. The organic phase was dried (Na2SO4) and evaporated. The crude was purified by flash chromatography with ethyl acetate-petroleum ether (7-3) to give 17 mg of the title compound (50% yield).

후처리

  1. washthe solution was washed with aqueous saturated NaHCO3 solution
  2. dry with materialThe organic phase was dried (Na2SO4)
  3. customevaporated
  4. customThe crude was purified by flash chromatography with ethyl acetate-petroleum ether (7-3)

출처 및 근거

ORD 기록
ord-6cb627a6ee604040bc5f5bdbf9aeff00
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727988B2

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