Water → 5-Chloro-2-(5-(2-pyridyloxy)pentylthio)benzimidazole

HRID 1005955노트

반응식

HRID 1005955 반응식
S(O[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=1)(C1C=CC(C)=CC=1)(=O)=O.[Cl:24][C:25]1[CH:34]=[CH:33][C:28]2[N:29]=[C:30]([SH:32])[NH:31][C:27]=2[CH:26]=1.C(N(CC)CC)C.O>C(#N)C>[Cl:24][C:25]1[CH:34]=[CH:33][C:28]2[N:29]=[C:30]([S:32][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][O:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][N:19]=3)[NH:31][C:27]=2[CH:26]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 121371192-(5-Tosyloxy-pentyloxy)pyridineHCID 178527787HCID 178527787, 화합물

생성물 1

HCID 121371205-Chloro-2-(5-(2-pyridyloxy)pentylthio)benzimidazole수율 42%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

0.67 g of the compound obtained in Example 3b and 0.37 g of 5-chloro-2-mercaptobenzimidazole were refluxed for 5 hours in 15 ml of acetonitrile containing 0.25 g of triethylamine. The reaction mixture was cooled to room temperature, then added with water and extracted with ethyl acetate. The extract was dried over sodium sulfate and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane) to obtain 0.25 g of the title compound (yield: 42%).

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe extract was dried over sodium sulfate
  3. customthe solvent was evaporated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane)

출처 및 근거

ORD 기록
ord-a0a782bd816b4f42b245bfcaa813e2dd
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787561B1

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