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

HRID 230851노트

반응식

HRID 230851 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-15e3655b520144ca863276a4bcec9132
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566786B2

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