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Iodide Ion → 7-(1-Ethylpropyl)-4-methoxy-1-methyl-1,3-dihydro-2H-benzimidazol-2-one

HRID 1698560
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반응식

HRID 1698560 반응식
Br[C:2]1[C:10]2[NH:9][C:8](=[O:11])[N:7]([CH3:12])[C:6]=2[C:5]([CH:13]([CH2:16][CH3:17])[CH2:14][CH3:15])=[CH:4][CH:3]=1.[I-].[CH3:19][O-:20].[Na+]>CO.CN(C)C=O.O>[CH2:14]([CH:13]([C:5]1[C:6]2[N:7]([CH3:12])[C:8](=[O:11])[NH:9][C:10]=2[C:2]([O:20][CH3:19])=[CH:3][CH:4]=1)[CH2:16][CH3:17])[CH3:15]
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참가 물질

7

반응물 3

HCID 30165Iodide IonHCID 10942334Sodium MethoxideHCID 672727554-bromo-7-(1-ethylpropyl)-1-methyl-1,3-dihydro-2H-benzimidazol-2-one

생성물 1

HCID 672729917-(1-Ethylpropyl)-4-methoxy-1-methyl-1,3-dihydro-2H-benzimidazol-2-one수율 91%

시약·촉매·용매 3

HCID 887Methanol용매
HCID 962
Water
용매
HCID 6228Dimethylformamide용매

실험 절차

A solution of 4-bromo-7-(1-ethylpropyl)-1-methyl-1,3-dihydro-2H-benzimidazol-2-one (250 mg, 0.841 mmol), anhydrous cuprus iodide (192 mg, 1.01 mmol) and 28% sodium methoxide in methanol (5.2 mL) in N,N-dimethylformamide (5 mL) was heated at 100° C. for 1 h. After cooling, the mixture was diluted with water and extracted with ethyl acetate. The organics were dried over magnesium sulfate, filtered and concentrated in vacuo to give the title compound (190 mg, 0.765 mmol, 91%).

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organics were dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a595cf219eb44013b2a5e68d7db1fa46
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08163935B2

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