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

HRID 1005955ノート

反応式

HRID 1005955 の反応式
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

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 121371192-(5-Tosyloxy-pentyloxy)pyridineHCID 178527787HCID 178527787、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-a0a782bd816b4f42b245bfcaa813e2dd
出典データセット
uspto-grants-2004_09
特許番号
US06787561B1

反応ノート

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