Methyl iodide → 4-[2,5-Dioxo-4-hydroxymethyl-3-methyl-4-phenylimidazolidin-1-yl]-2-methoxybenzonitrile

HRID 389907노트

반응식

HRID 389907 반응식
[C:1](=O)([O-])[O-].[K+].[K+].CI.[O:9]=[C:10]1[NH:14][C:13]([CH2:21][OH:22])([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:12](=[O:23])[N:11]1[C:24]1[CH:31]=[CH:30][C:27]([C:28]#[N:29])=[C:26]([O:32][CH3:33])[CH:25]=1>CN(C=O)C>[O:9]=[C:10]1[N:14]([CH3:1])[C:13]([CH2:21][OH:22])([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)[C:12](=[O:23])[N:11]1[C:24]1[CH:31]=[CH:30][C:27]([C:28]#[N:29])=[C:26]([O:32][CH3:33])[CH:25]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 671311834-[2,5-Dioxo-4-hydroxymethyl-4-phenylimidazolidin-1-yl]-2-methoxybenzonitrile

생성물 1

HCID 593171894-[2,5-Dioxo-4-hydroxymethyl-3-methyl-4-phenylimidazolidin-1-yl]-2-methoxybenzonitrile

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

173 mg potassium carbonate and 86 μL methyl iodide are added to a solution of 141 mg 4-[2,5-dioxo-4-hydroxymethyl-4-phenylimidazolidin-1-yl]-2-methoxybenzonitrile in 2 mL DMF. The mixture is stirred overnight at room temperature, evaporated to dryness, The residue is taken in water and extracted with ethyl acetate. The organic layer is dried over magnesium sulfate, filtered, evaporated and chromatographed over silica gel while eluting with 70/30 heptane/ethyl acetate mixture to give the expected product.

후처리

  1. customevaporated to dryness
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer is dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customchromatographed over silica gel
  7. washwhile eluting with 70/30 heptane/ethyl acetate mixture

출처 및 근거

ORD 기록
ord-3333604f259d48adae99c03adf1f45f5
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08383608B2

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