Chloroform → 1H-Benzimidazol-6-amine,1,2-dimethyl-(9CI)

HRID 230851ノート

反応式

HRID 230851 の反応式
O.O.[Sn](Cl)Cl.[CH3:6][N:7]1[C:11]2[CH:12]=[C:13]([N+:16]([O-])=O)[CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[CH3:19].C(Cl)(Cl)Cl.[OH-].[Na+]>Cl>[CH3:6][N:7]1[C:11]2[CH:12]=[C:13]([NH2:16])[CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[CH3:19]

参加物

6

反応物 4

HCID 6212ChloroformHCID 14798Sodium HydroxideHCID 61436Stannous chloride dihydrateHCID 133278651,2-dimethyl-6-nitro-1H-benzo[d]imidazole

生成物 1

HCID 122280631H-Benzimidazol-6-amine,1,2-dimethyl-(9CI)

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

To a stirred solution of tin (II) chloride dihydrate (4.7 g) in concentrated hydrochloric acid (15 ml) was added 1,2-dimethyl-6-nitro-1H-benzimidazole (1 g) (J. Chem. Soc.,1931, 1143-1153), and the mixture was stirred at room temperature for 6 h. The mixture was poured onto ice and chloroform, and basified to pH 10 by the addition of 10M sodium hydroxide solution. The mixture was extracted several times with chloroform and the combined organic extracts dried and concentrated in vacuo to give a brown solid. This was crystallised from ethanol to give the title compound.

後処理

  1. extractionThe mixture was extracted several times with chloroform
  2. customthe combined organic extracts dried
  3. concentrationconcentrated in vacuo
  4. customto give a brown solid
  5. customThis was crystallised from ethanol

出典と根拠

ORDレコード
ord-15e3655b520144ca863276a4bcec9132
出典データセット
uspto-grants-2009_07
特許番号
US07566786B2

反応ノート

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