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Methyl iodide → HCID 18960747, 화합물

HRID 1708324
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HRID 1708324 반응식
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[CH:30]=[CH:29][C:9]([C:10]([N:12]2[CH2:17][CH2:16][CH:15]([N:18]3[C:28]4[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=4)[CH2:22][CH2:21][C:19]3=[O:20])[CH2:14][CH2:13]2)=[O:11])=[CH:8][CH:7]=1.[C:31](=O)([O-])[O-].[K+].[K+].CI>CN(C)C=O>[CH3:31][N:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[CH:30]=[CH:29][C:9]([C:10]([N:12]2[CH2:13][CH2:14][CH:15]([N:18]3[C:28]4[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=4)[CH2:22][CH2:21][C:19]3=[O:20])[CH2:16][CH2:17]2)=[O:11])=[CH:8][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodide2회HCID 11430Potassium Carbonate2회HCID 18960751HCID 18960751, 화합물

생성물 1

HCID 18960747HCID 18960747, 화합물수율 14.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 1-{1-[4-(2-imidazolyl)benzoyl]-4-piperidinyl}-3,4-dihydrocarbostyril (1.0 g) and potassium carbonate (0.35 g) in dimethylformamide (10 ml) is added methyl iodide (0.16 ml) under ice-cooling, and the mixture is stirred at room temperature overnight. Further, to the mixture are added methyl iodide (0.16 ml) and potassium carbonate (0.3 g), and the mixture is stirred at room temperature for 8 hours. The mixture is poured into ice-water, extracted with ethyl acetate, washed with water and dried over sodium sulfate. After concentrated under reduced pressure, the resulting residue is purified by silica gel column chromatography (eluent; dichloromethane:methanol=25:1) and recrystallized from ethyl acetate to give 1-{1-[4-(1-methyl-2-imidazolyl)benzoyl]-4-piperidinyl}-3,4-dihydrocarbostyril (0.15 g) as colorless scales, m.p. 177°-179° C.

후처리

  1. temperaturecooling
  2. stirringthe mixture is stirred at room temperature for 8 hours
  3. extractionextracted with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationAfter concentrated under reduced pressure
  7. customthe resulting residue is purified by silica gel column chromatography (eluent; dichloromethane:methanol=25:1)
  8. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-65fec4ef612e493f8fbe3114d01082a8
출처 데이터셋
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05356904

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