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

HRID 558962노트

반응식

HRID 558962 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 10313229titanium(III) trichloride촉매HCID 887Methanol용매HCID 962Water용매2회

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-06d76078b39e45029c0bf77efcd7ed01
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063038B2

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