Dimethylformamide → 2,3-bis(4-methoxyphenyl)-6,7-dihydro-5H-pyrrolo[1,2-a]imidazole

HRID 2052679ノート

反応式

HRID 2052679 の反応式
CN(C)C=O.Br[CH:7]([C:18]1[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=1)[C:8]([C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=1)=O.[NH2:26][C:27]1[CH2:31][CH2:30][CH2:29][N:28]=1>O>[CH3:17][O:16][C:13]1[CH:14]=[CH:15][C:10]([C:8]2[N:26]=[C:27]3[CH2:31][CH2:30][CH2:29][N:28]3[C:7]=2[C:18]2[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=2)=[CH:11][CH:12]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 3441532-Bromo-1,2-bis(4-methoxyphenyl)ethanoneHCID 127789042-Amino-1-pyrroline

生成物 1

HCID 12815562,3-bis(4-methoxyphenyl)-6,7-dihydro-5H-pyrrolo[1,2-a]imidazole

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 300 ml of dry N,N-dimethylformamide was added 30. g (0.09 mol) of 2-bromo-1,2-di(4-methoxyphenyl)ethanone and 19.5 g (0.27 mol) of 2-amino-4,5-dihydro-3H-pyrrole. The mixture was stirred for three days at 25° with the exclusion of moisture. The reaction mixture was poured into water and the aqueous suspension was extracted three times with methylene chloride. The organic extracts were combined and washed six times with water, then dried (K2CO3). The solvent was evaporated and the residue was recrystallized from chloroform-hexane and dried overnight (80° in vacuo) to give the title compound, m.p. 146°-147.5°.

後処理

  1. extractionthe aqueous suspension was extracted three times with methylene chloride
  2. washwashed six times with water
  3. dry with materialdried (K2CO3)
  4. customThe solvent was evaporated
  5. customthe residue was recrystallized from chloroform-hexane
  6. customdried overnight (80° in vacuo)

出典と根拠

ORDレコード
ord-08191bfd8ed249808f2354f250ab9e8a
出典データセット
uspto-grants-1980_01
特許番号
US04186205

反応ノート

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