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Hydrochloric Acid → HCID 59403298、化合物

HRID 1873866
ノート
印刷プレビュー

反応式

HRID 1873866 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 59403300HCID 59403300、化合物

生成物 1

HCID 59403298HCID 59403298、化合物収率 100.3%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-844c5b0158204b7fa218af69ab350df5
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08304444B2

反応ノート

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