Triethylamine → HCID 22662877, 화합물

HRID 43501노트

반응식

HRID 43501 반응식
[OH:1][CH2:2][C:3]1[N:4]=[CH:5][NH:6][C:7]=1[CH3:8].C(N(CC)CC)C.[Si:16](Cl)([C:19]([CH3:22])([CH3:21])[CH3:20])([CH3:18])[CH3:17].C(OCC)(=O)C>CN(C=O)C>[Si:16]([O:1][CH2:2][C:3]1[N:4]=[CH:5][NH:6][C:7]=1[CH3:8])([C:19]([CH3:22])([CH3:21])[CH3:20])([CH3:18])[CH3:17]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 28928tert-Butyldimethylsilyl chlorideHCID 1224334-hydroxymethyl-5-methyl-1H-imidazole

생성물 1

HCID 22662877HCID 22662877, 화합물수율 77%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-(Hydroxymethyl)-5-methyl-1H-imidazole (4 g, 26.9 mmol) was dissolved in DMF (80 mL). Triethylamine (13.5 mL, 96.9 mmol) and tert-butyl(dimethyl)silyl chloride (4.68 g, 31.0 mmol) were added, followed by stirring for three hours. Ethyl acetate was added to the reaction solution, and the organic layer was washed with brine and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=4/1, dichloromethane/methanol=92/8) to obtain 4.67 g of the title compound (77%).

후처리

  1. washthe organic layer was washed with brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentration under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=4/1, dichloromethane/methanol=92/8)

출처 및 근거

ORD 기록
ord-4b12e4695cd24b6ab86a97e8736a2e67
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536197B2

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