Sodium Acetate → N*2*-tert-Butyl-3-chlorobenzene-1,2-diamine

HRID 558962ノート

反応式

HRID 558962 の反応式
[C:1]([NH:5][C:6]1[C:11]([N+:12]([O-])=O)=[CH:10][CH:9]=[CH:8][C:7]=1[Cl:15])([CH3:4])([CH3:3])[CH3:2].C([O-])(=O)C.[Na+]>CO.O.[Cl-].[Ti+3].[Cl-].[Cl-]>[C:1]([NH:5][C:6]1[C:11]([NH2:12])=[CH:10][CH:9]=[CH:8][C:7]=1[Cl:15])([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 2

HCID 517045Sodium AcetateHCID 10823273N-tert-Butyl-6-chloro-2-nitroaniline

生成物 1

HCID 10845671N*2*-tert-Butyl-3-chlorobenzene-1,2-diamine

試薬・触媒・溶媒 3

HCID 10313229titanium(III) trichloride触媒HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

A solution of titanium (III) chloride (10 wt. % in 20-30% hydrochloric acid, 120 ml, 78 mmol) was added drop wise to a solution of tert-butyl-(2-chloro-6-nitrophenyl)-amine from Example 12A (5.7 g, 25 mmol) and sodium acetate (112 g, 1.4 moles) in methanol (205 ml) and water (63 ml). The mixture was stirred for 2 h, water was added to dissolve remaining solids and the organic solvent was evaporated. The mixture was neutralised with solid sodium hydrogen carbonate and extracted with EtOAc. The organic extracts were dried and evaporated to afford an orange oil; yield 4.7 g, 94%.

後処理

  1. dissolutionto dissolve
  2. customthe organic solvent was evaporated
  3. extractionextracted with EtOAc
  4. customThe organic extracts were dried
  5. customevaporated
  6. customto afford an orange oil

出典と根拠

ORDレコード
ord-06d76078b39e45029c0bf77efcd7ed01
出典データセット
uspto-grants-2011_11
特許番号
US08063038B2

反応ノート

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