Methyl iodide → HCID 19866681, 화합물

HRID 1199464노트

반응식

HRID 1199464 반응식
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[NH:13][C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=2[N:10]=1.CI.[C:20](=O)([O-])[O-].[K+].[K+]>CN(C)C=O.[Cl-].[Na+].O>[CH3:20][N:13]1[C:12]2[CH:14]=[CH:15][CH:16]=[CH:17][C:11]=2[N:10]=[C:9]1[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[S:2][CH3:1]

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 123160831H-Benzimidazole, 2-[2-(methylthio)phenyl]-

생성물 1

HCID 19866681HCID 19866681, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 57417360Sodium chloride; water용매

실험 절차

The product of step (a) above (3.25 g), methyl iodide (1.92 g) and potassium carbonate (5.2 g) were stirred together in dry dimethylformamide (50 ml) at room temperature for 24 hours. The reaction mixture was poured into brine and extracted into ethyl acetate, the extract was washed with excess brine, dried over magnesium sulphate and evaporated to dryness in vacuo and the residue was purified by flash chromatography (SiO2 /CH2Cl2 9:1 ethyl acetate) to afford the sub-title compound as yellow solid, MS MW 254 bp 239.

후처리

  1. extractionextracted into ethyl acetate
  2. washthe extract was washed with excess brine
  3. dry with materialdried over magnesium sulphate
  4. customevaporated to dryness in vacuo
  5. customthe residue was purified by flash chromatography (SiO2 /CH2Cl2 9:1 ethyl acetate)

출처 및 근거

ORD 기록
ord-42976fe0c28b40e28a0f396355ff0402
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04900751

반응 노트

불러오는 중…