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Water → 4-benzyloxy-1-methyl-2-dimethylamino-1H-benzimidazole

HRID 636502
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HRID 636502 반응식
[CH2:1]([O:8][C:9]1[C:17]2[N:16]=[C:15]([NH:18][CH3:19])[N:14]([CH3:20])[C:13]=2[CH:12]=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH3:23]I.O>CN(C)C=O>[CH2:1]([O:8][C:9]1[C:17]2[N:16]=[C:15]([N:18]([CH3:23])[CH3:19])[N:14]([CH3:20])[C:13]=2[CH:12]=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 106594804-benzyloxy-1-methyl-2-methylamino-1H-benzimidazole

생성물 1

HCID 106842294-benzyloxy-1-methyl-2-dimethylamino-1H-benzimidazole수율 47.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

To a solution of 4-benzyloxy-1-methyl-2-methylamino-1H-benzimidazole (200 mg) in dimethylformamide (2 ml) was added sodium hydride (32.9 mg) under ice-cooling, and the mixture was stirred for 15 minutes. To the mixture was added methyl iodide (127 mg), and the mixture was stirred for 15 minutes under ice-cooling and then for 2 hours at ambient temperature. Water was added to the reaction mixture, and extracted with chloroform. The organic layer was dried over magnesium sulfate and evaporated in vacuo. The residue was purified by flash chromatography (chloroform:methanol=50:1, v/v) to give 4-benzyloxy-1-methyl-2-dimethylamino-1H-benzimidazole (100 mg).

후처리

  1. temperaturecooling
  2. stirringthe mixture was stirred for 15 minutes under ice-
  3. temperaturecooling
  4. waitfor 2 hours at ambient temperature
  5. extractionextracted with chloroform
  6. dry with materialThe organic layer was dried over magnesium sulfate
  7. customevaporated in vacuo
  8. customThe residue was purified by flash chromatography (chloroform

출처 및 근거

ORD 기록
ord-cd427960f30f46b4a0720bcacabe6ebe
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06194396B1

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