Stannous Chloride → 1-(3-Amino-3-methyl-butyl)-5-methoxy-3-methyl-1,3-dihydro-benzimidazol-2-one

HRID 33393노트

반응식

HRID 33393 반응식
[CH3:1][O:2][C:3]1[CH:21]=[CH:20][C:6]2[N:7]([CH2:12][CH2:13][C:14]([CH3:19])([N+:16]([O-])=O)[CH3:15])[C:8](=[O:11])[N:9]([CH3:10])[C:5]=2[CH:4]=1.Cl[Sn]Cl>C(O)C>[NH2:16][C:14]([CH3:19])([CH3:15])[CH2:13][CH2:12][N:7]1[C:6]2[CH:20]=[CH:21][C:3]([O:2][CH3:1])=[CH:4][C:5]=2[N:9]([CH3:10])[C:8]1=[O:11]

참가 물질

4

반응물 2

HCID 24479Stannous ChlorideHCID 671887485-Methoxy-3-methyl-1-(3-methyl-3-nitro-butyl)-1,3-dihydro-benzimidazol-2-one

생성물 1

HCID 671880221-(3-Amino-3-methyl-butyl)-5-methoxy-3-methyl-1,3-dihydro-benzimidazol-2-one

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2.7 g (8.7 mmol) 5-methoxy-3-methyl-1-(3-methyl-3-nitro-butyl)-1,3-dihydro-benzimidazol-2-one and 9.93 g (44.0 mmol) SnCl2 2H2O in 200 mL ethanol are refluxed for 3 hours. The reaction mixture is evaporated down, combined with sodium carbonate solution and filtered. The filtrate is extracted with ethyl acetate and the combined organic phases are washed with water, dried and freed from the solvent. The residue is dissolved in ethanol and the solution is combined with ethereal hydrochloric acid. After the solvent has been distilled off the solid remaining is stirred with diisopropylether.

후처리

  1. customThe reaction mixture is evaporated down
  2. filtrationfiltered
  3. extractionThe filtrate is extracted with ethyl acetate
  4. washthe combined organic phases are washed with water
  5. customdried
  6. dissolutionThe residue is dissolved in ethanol
  7. distillationAfter the solvent has been distilled off the solid

출처 및 근거

ORD 기록
ord-275ab9c9744849938acbd953b0b242af
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429583B2

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