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Hydrochloric Acid → HCID 59403298, 화합물

HRID 1873866
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HRID 1873866 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH:9]([NH:15][O:16][CH3:17])[CH:10]([N+:12]([O-])=O)[CH3:11].Cl>[Zn].CC(O)C>[NH2:12][CH:10]([CH3:11])[CH:9]([NH:15][O:16][CH3:17])[C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[Cl:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 59403300HCID 59403300, 화합물

생성물 1

HCID 59403298HCID 59403298, 화합물수율 100.3%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 3776Isopropanol용매

실험 절차

N-[1-(2,4-dichloro-phenyl)-2-nitro-propyl]-O-methyl-hydroxylamine (0.123 g, 0.44 mmol), was dissolved with i-PrOH (9 ml) and treated with 1N HCl (4.4 ml, 4.4 mmol). Zinc dust (0.58 g, 8.8 mmol) was then added in small portions over 15 minutes and the solution allowed to stir for two hours at ambient temperature. The suspension was quenched by addition of saturated NaHCO3 (15 ml), stirred for 15 minutes and filtered through a small plug of Celite, washing with ethylacetate (40 ml). The organic extract was separated, dried over anhydrous MgSO4 an filtered and the solvent was removed under reduced pressure. 110 mg (100% of theory) of N-[2-Amino-1-(2,4-dichloro-phenyl)-propyl]-O-methyl-hydroxylamine (compound Z1.14) was obtained in the form of a colourless oil as a mixture of diastereomeres.

후처리

  1. customThe suspension was quenched by addition of saturated NaHCO3 (15 ml)
  2. stirringstirred for 15 minutes
  3. filtrationfiltered through a small plug of Celite
  4. washwashing with ethylacetate (40 ml)
  5. extractionThe organic extract
  6. customwas separated
  7. dry with materialdried over anhydrous MgSO4
  8. filtrationan filtered
  9. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-844c5b0158204b7fa218af69ab350df5
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08304444B2

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