N-Benzyl-N,2-dimethyl-5-nitro-aniline → HCID 55091508、化合物

HRID 2242045ノート

反応式

HRID 2242045 の反応式
[CH2:1]([N:8]([CH3:19])[C:9]1[CH:14]=[C:13]([N+:15]([O-])=O)[CH:12]=[CH:11][C:10]=1[CH3:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>CO.Cl>[CH2:1]([N:8]([CH3:19])[C:9]1[CH:14]=[C:13]([NH2:15])[CH:12]=[CH:11][C:10]=1[CH3:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 1

HCID 66915963N-Benzyl-N,2-dimethyl-5-nitro-aniline

生成物 1

HCID 55091508HCID 55091508、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒

実験手順

SnCl2-dihydrate (1117 mg, 4.95 mmol) is added to a solution of N-Benzyl-N,2-dimethyl-5-nitro-aniline (247 mg, 0.96 mmol) in methanol (10 mL) and conc. HCl (1 mL). After boiling under reflux for 2.5 h, volatiles are evaporated under reduced pressure and the residue is partitioned between EtOAc and water, the pH being adjusted to approx. 10 by the addition of 2N NaOH. The organic layer is washed with sat. brine, dried (Na2SO4), and evaporated. Chromatography of the residue (silica gel, hexanes/EtOAc 3:2) yields N3-benzyl-N3,4-dimethyl-benzene-1,3-diamine

後処理

  1. temperatureunder reflux for 2.5 h
  2. customvolatiles are evaporated under reduced pressure
  3. customthe residue is partitioned between EtOAc and water
  4. additionby the addition of 2N NaOH
  5. washThe organic layer is washed with sat. brine
  6. dry with materialdried (Na2SO4)
  7. customevaporated

出典と根拠

ORDレコード
ord-814472ea39ec4781925da15ab276aa24
出典データセット
uspto-grants-2010_03
特許番号
US07671063B2

反応ノート

読み込み中…