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

HRID 258846

반응식

HRID 258846 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-694125e3bfad4e168ff476ac012846e7
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04035369

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