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1-[2-[4-(2-Methoxycarbonyl-2-methylpropyl)phenyl]ethyl]-1,5-diazacyclooctane → 1-[1-(4-chlorophenylmethyl)-1H-benzimidazol-2-yl]-5-[2-[4-(2-methoxycarbonyl-2-methylpropyl)phenyl]ethyl]-1,5-diazacyclooctane

HRID 55331
ノート
印刷プレビュー

反応式

HRID 55331 の反応式
Br[C:2]1[N:6]([CH2:7][C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)[C:5]2[CH:15]=[CH:16][CH:17]=[CH:18][C:4]=2[N:3]=1.[CH3:19][O:20][C:21]([C:23]([CH3:42])([CH3:41])[CH2:24][C:25]1[CH:30]=[CH:29][C:28]([CH2:31][CH2:32][N:33]2[CH2:40][CH2:39][CH2:38][NH:37][CH2:36][CH2:35][CH2:34]2)=[CH:27][CH:26]=1)=[O:22]>C(O)CCC>[Cl:14][C:11]1[CH:12]=[CH:13][C:8]([CH2:7][N:6]2[C:5]3[CH:15]=[CH:16][CH:17]=[CH:18][C:4]=3[N:3]=[C:2]2[N:37]2[CH2:38][CH2:39][CH2:40][N:33]([CH2:32][CH2:31][C:28]3[CH:29]=[CH:30][C:25]([CH2:24][C:23]([C:21]([O:20][CH3:19])=[O:22])([CH3:42])[CH3:41])=[CH:26][CH:27]=3)[CH2:34][CH2:35][CH2:36]2)=[CH:9][CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 199575131-[2-[4-(2-Methoxycarbonyl-2-methylpropyl)phenyl]ethyl]-1,5-diazacyclooctaneHCID 199575172-bromo-1-(4-chlorophenylmethyl)-1H-benzimidazole

生成物 1

HCID 199575141-[1-(4-chlorophenylmethyl)-1H-benzimidazol-2-yl]-5-[2-[4-(2-methoxycarbonyl-2-methylpropyl)phenyl]ethyl]-1,5-diazacyclooctane収率 58%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

To a solution of 2-bromo-1-(4-chlorophenylmethyl)-1H-benzimidazole (0.029 g) in n-butanol (0.5 ml) was added 1-[2-[4-(2-methoxycarbonyl-2-methylpropyl)phenyl]ethyl]-1,5-diazacyclooctane (0.102 g), and the mixture was refluxed for 3 hours. The reaction mixture was quenched with a saturated aqueous NaHCO3 solution (30 ml), and the mixture was extracted with methylene chloride (20 ml). The extract was washed with water, and dried over anhydrous MgSO4. The solvent was removed under reduced pressure, and the residue was purified by medium pressure liquid column chromatography on a silica gel column using a mixture of methylene chloride, diethyl ether and methanol (1:1:0.2) as eluent to give 1-[1-(4-chlorophenylmethyl)-1H-benzimidazol-2-yl]-5-[2-[4-(2-methoxycarbonyl-2-methylpropyl)phenyl]ethyl]-1,5-diazacyclooctane (0.030 g) as a colorless oily liquid.

後処理

  1. temperaturethe mixture was refluxed for 3 hours
  2. customThe reaction mixture was quenched with a saturated aqueous NaHCO3 solution (30 ml)
  3. extractionthe mixture was extracted with methylene chloride (20 ml)
  4. washThe extract was washed with water
  5. dry with materialdried over anhydrous MgSO4
  6. customThe solvent was removed under reduced pressure
  7. customthe residue was purified by medium pressure liquid column chromatography on a silica gel column
  8. additiona mixture of methylene chloride, diethyl ether and methanol (1:1:0.2) as eluent

出典と根拠

ORDレコード
ord-e73b6b9de0744504bd3c6e59ec7f1560
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05624948

反応ノート

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