2-Nitroaniline → 4-Tert-octyl-2-nitroaniline

HRID 231635

반응식

HRID 231635 반응식
[N+:1]([C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH2:6])([O-:3])=[O:2].[CH3:11][C:12]([CH2:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[CH2:13]>[Cl-].[Zn+2].[Cl-]>[C:12]([C:9]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([N+:1]([O-:3])=[O:2])[CH:10]=1)([CH2:14][C:15]([CH3:18])([CH3:17])[CH3:16])([CH3:13])[CH3:11]

참가 물질

4

반응물 2

HCID 69462-Nitroaniline2회HCID 78682,4,4-Trimethyl-1-pentene

생성물 1

HCID 141221784-Tert-octyl-2-nitroaniline

시약·촉매·용매 1

HCID 3007855Zincchloride촉매

반응 조건

온도
60 °C

실험 절차

In a 2-liter reaction flask fitted with a condenser, nitrogen inlet, stirrer, thermometer and addition funnel is placed 272 grams (2.0 moles) of anhydrous zinc chloride. The flask is placed under a nitrogen atmosphere and 166 ml (2.0 moles) of concentrated (12N) hydrochloric acid is added over a 10-minute period with the temperature rising from 22° to 40° C. To this is then added 276 grams (2.0 moles) of o-nitroaniline over a 15-minute period to avoid the formation of lumps. The resulting thick red slurry is heated to 60° C. and then 474 grams (3.0 moles) of diisobutylene is added gradually over a 110-minute period with the temperature rising during this period from 60° to 90° C. The deep red fluid reaction mixture is heated for another 18 hours at reflux till only a trace of o-nitroaniline is observed by thin layer chromatography.

후처리

  1. customIn a 2-liter reaction flask
  2. customfitted with a condenser, nitrogen inlet, stirrer
  3. additionthermometer and addition funnel
  4. concentration166 ml (2.0 moles) of concentrated (12N) hydrochloric acid
  5. additionis added over a 10-minute period with the temperature
  6. customrising from 22° to 40° C
  7. waitrising during this period from 60° to 90° C
  8. customThe deep red fluid reaction mixture
  9. temperatureis heated for another 18 hours

출처 및 근거

ORD 기록
ord-7766e2995dfc4649b0ee45e4ed5658cc
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04847367

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