Ethyl 4-bromobutyrate → Ethyl 4-[(1H-benzimidazol-2-yl)sulfanyl]butanoate

HRID 893353ノート

反応式

HRID 893353 の反応式
[SH:1][C:2]1[NH:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[Na].Br[CH2:13][CH2:14][CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17]>C(O)C>[N:3]1[C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[NH:6][C:2]=1[S:1][CH2:13][CH2:14][CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17]

参加物

5

反応物 3

HCID 76300Ethyl 4-bromobutyrateHCID 5360545SodiumHCID 178527775HCID 178527775、化合物

生成物 1

HCID 12624992Ethyl 4-[(1H-benzimidazol-2-yl)sulfanyl]butanoate収率 97.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

50 g of 2-mercaptobenzimidazole are dissolved in 300 ml of ethanol, and a solution of 7.65 g of sodium in 150 ml of ethanol is added at room temperature, with stirring. The mixture is stirred for a few minutes at room temperature and 64.3 g of ethyl 4-bromobutyrate are added rapidly. The reaction mixture is refluxed for 6 hours and then cooled. The solvents are evaporated off to dryness under vacuum, the residue is taken up with water and the crystals obtained are filtered off, washed with water and then with ether and dried to give 85 g of ethyl 4-(benzimidazol-2-yl)mercaptobutanoate in the form of crystals melting at 70°-72° C.

後処理

  1. stirringThe mixture is stirred for a few minutes at room temperature
  2. temperatureThe reaction mixture is refluxed for 6 hours
  3. temperaturecooled
  4. customThe solvents are evaporated off to dryness under vacuum
  5. customthe crystals obtained
  6. filtrationare filtered off
  7. washwashed with water
  8. dry with materialwith ether and dried

出典と根拠

ORDレコード
ord-428f377e708d49baa00bc0a2df2e7fa7
出典データセット
uspto-grants-1992_06
特許番号
US05124336

反応ノート

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