Potassium Iodide → 8-[3-(1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one

HRID 46870

반응식

HRID 46870 반응식
Cl[CH2:2][CH2:3][CH2:4][N:5]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[NH:7][C:6]1=[O:14].[C:15]1([N:21]2[C:25]3([CH2:30][CH2:29][NH:28][CH2:27][CH2:26]3)[C:24](=[O:31])[NH:23][CH2:22]2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>O.CC(C)CC(=O)C>[O:14]=[C:6]1[N:5]([CH2:4][CH2:3][CH2:2][N:28]2[CH2:27][CH2:26][C:25]3([N:21]([C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=4)[CH2:22][NH:23][C:24]3=[O:31])[CH2:30][CH2:29]2)[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[NH:7]1

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 705561-Phenyl-1,3,8-triazaspiro(4.5)decan-4-oneHCID 18104191-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one

생성물 1

HCID 203855688-[3-(1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one수율 22%

시약·촉매·용매 2

HCID 962Water용매HCID 7909Methyl Isobutyl Ketone용매

실험 절차

A mixture of 2.3 parts of 1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one, 2.31 parts of 1-phenyl-1,3,8-triazaspiro-[4,5]decan-4-one, 3.2 parts of sodium carbonate, 0.1 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. After cooling to room temperature, water is added. The undissolved product is filtered off and purified by column-chromatography over silica gel using a mixture of trichloromethane and 10% of methanol as eluent. The pure fractions are collected and the eluent is evaporated, yielding 0.9 parts (22%) of 8-[3-(1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one; mp. 228° C.

후처리

  1. temperaturerefluxed overnight
  2. filtrationThe undissolved product is filtered off
  3. custompurified by column-chromatography over silica gel using
  4. additiona mixture of trichloromethane and 10% of methanol as eluent
  5. customThe pure fractions are collected
  6. customthe eluent is evaporated

출처 및 근거

ORD 기록
ord-0b20b498803e49308aa1de366ef75836
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04175129

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