Sodium Carbonate → 2-Aminobenzimidazole

HRID 2166126ノート

反応式

HRID 2166126 の反応式
ClCCOCC.Br.Br.N1CCC([NH:15][C:16]2[NH:20][C:19]3[CH:21]=[CH:22][CH:23]=[CH:24][C:18]=3[N:17]=2)CC1.C(=O)([O-])[O-].[Na+].[Na+].CN(C)C(=O)C>O>[NH:17]1[C:18]2[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=2[N:20]=[C:16]1[NH2:15]

参加物

6

反応物 4

HCID 10340Sodium CarbonateHCID 12341Ethane, 1-chloro-2-ethoxy-HCID 31374DimethylacetamideHCID 22036968N-(Piperidin-4-yl)-1H-benzo[d]imidazol-2-amine dihydrobromide

生成物 1

HCID 136242-Aminobenzimidazole

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

A mixture of 32 parts of 1-chloro-2-ethoxyethane, 94.5parts of N-(4-piperidinyl)-1H-benzimidazol-2-amine dihydrobromide, 90 parts of sodium carbonate and 540 parts of N,N-dimethylacetamide was stirred overnight at 70° C. After cooling, the reaction mixture was poured into water. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was boiled in acetonitrile. After cooling, the precipitated product was filtered off and dried, yielding 42.4 parts (58.8%) of N-[1-(2-ethoxyethyl)-4-piperidinyl[-1H-benzimidazol-2-amine; mp. 212° C. (interm. 29).

後処理

  1. temperatureAfter cooling
  2. extractionThe product was extracted with dichloromethane
  3. customThe extract was dried
  4. filtrationfiltered
  5. customevaporated
  6. temperatureAfter cooling
  7. filtrationthe precipitated product was filtered off
  8. customdried

出典と根拠

ORDレコード
ord-a2dada330cdf4c488f3c7bb0c55e1fe3
出典データセット
uspto-grants-1990_07
特許番号
US04943580

反応ノート

読み込み中…