1,1'-Carbonyldiimidazole → 1H-Imidazole-1-carboxamide, N-(2,2-dimethoxyethyl)-

HRID 1604428ノート

反応式

HRID 1604428 の反応式
[C:1](N1C=CN=C1)([N:3]1[CH:7]=[CH:6][N:5]=[CH:4]1)=[O:2].[CH3:13][O:14][CH:15]([O:18][CH3:19])[CH2:16][NH2:17]>C(Cl)Cl>[CH3:13][O:14][CH:15]([O:18][CH3:19])[CH2:16][NH:17][C:1]([N:3]1[CH:7]=[CH:6][N:5]=[CH:4]1)=[O:2]

参加物

4

反応物 2

HCID 682631,1'-CarbonyldiimidazoleHCID 89728Aminoacetaldehyde dimethyl acetal

生成物 1

HCID 187633681H-Imidazole-1-carboxamide, N-(2,2-dimethoxyethyl)-収率 69%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A suspension of 1,1'-carbonyldiimidazole (162.15 g) in CH2Cl2 (500 ml) was stirred on an ice-bath. 2,2-Dimethoxyethanamine (105.14 g) was added dropwise and the resulting reaction solution was stirred for 16 hours. The reaction mixture was cooled on ice, stirred for 30 minutes, and was allowed to crystallize. The precipitate was filtered off, stirred for 15 minutes in ethylacetate (250 ml) at RT, then cooled on an ice-bath for 30 minutes. The precipitate was filtered off, washed twice with DIPE (50 ml), then dried, yielding 137.4 g (69%) of N-(2,2-dimethoxyethyl)-1-H-imidazole-1-carboxamide (interm. 26).

後処理

  1. customthe resulting reaction solution
  2. stirringwas stirred for 16 hours
  3. temperatureThe reaction mixture was cooled on ice
  4. stirringstirred for 30 minutes
  5. customto crystallize
  6. filtrationThe precipitate was filtered off
  7. stirringstirred for 15 minutes in ethylacetate (250 ml) at RT
  8. temperaturecooled on an ice-bath for 30 minutes
  9. filtrationThe precipitate was filtered off
  10. washwashed twice with DIPE (50 ml)
  11. customdried

出典と根拠

ORDレコード
ord-1d50e98925a5462b937ba53c79bac68e
出典データセット
uspto-grants-1999_11
特許番号
US05994376

反応ノート

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