Methyl Isobutyl Ketone → 1-(3-chloropropyl)-2-(methylthio)-1H-benzimidazole

HRID 258846ノート

反応式

HRID 258846 の反応式
[CH3:1][S:2][C:3]1[NH:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[N:4]=1.Br[CH2:13][CH2:14][CH2:15][Cl:16].C(=O)([O-])[O-].[Na+].[Na+].CC(C)CC(=O)C>O>[Cl:16][CH2:15][CH2:14][CH2:13][N:7]1[C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[N:4]=[C:3]1[S:2][CH3:1]

参加物

6

反応物 4

HCID 7909Methyl Isobutyl KetoneHCID 80061-Bromo-3-chloropropaneHCID 10340Sodium CarbonateHCID 235392-(Methylthio)benzimidazole

生成物 1

HCID 135640281-(3-chloropropyl)-2-(methylthio)-1H-benzimidazole収率 50%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 8.2 parts of 2-(methylthio)-1H-benzimidazole, 16 parts of 1-bromo-3-chloropropane, 5.3 parts of sodium carbonate and 200 parts of 4-methyl-2-pentanone is stirred and refluxed for 44 hours. After cooling, water is added and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is stirred in 2,2'-oxybispropane. The unreacted starting material is filtered off and the filtrate is evaporated, yielding 6 parts (50%) of 1-(3-chloropropyl)-2-(methylthio)-1H-benzimidazole as an oily residue.

後処理

  1. temperaturerefluxed for 44 hours
  2. temperatureAfter cooling
  3. customthe layers are separated
  4. customThe organic phase is dried
  5. filtrationfiltered
  6. customevaporated
  7. stirringThe residue is stirred in 2,2'-oxybispropane
  8. filtrationis filtered off
  9. customthe filtrate is evaporated

出典と根拠

ORDレコード
ord-694125e3bfad4e168ff476ac012846e7
出典データセット
uspto-grants-1977_07
特許番号
US04035369

反応ノート

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