Dimethylamine → 4-tert-Butyl-N,N-dimethyl-2,6-dinitroaniline

HRID 1678834노트

반응식

HRID 1678834 반응식
[N+:1]([C:4]1[CH:9]=[C:8]([C:10]([CH3:13])([CH3:12])[CH3:11])[CH:7]=[C:6]([N+:14]([O-:16])=[O:15])[C:5]=1Cl)([O-:3])=[O:2].[CH3:18][NH:19][CH3:20].C(O)C>O>[CH3:18][N:19]([CH3:20])[C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:9][C:8]([C:10]([CH3:13])([CH3:12])[CH3:11])=[CH:7][C:6]=1[N+:14]([O-:16])=[O:15]

참가 물질

5

반응물 3

HCID 674DimethylamineHCID 702EthanolHCID 751764-tert-Butyl-2,6-dinitrochlorobenzene

생성물 1

HCID 203642434-tert-Butyl-N,N-dimethyl-2,6-dinitroaniline

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Two and six-tenths grams (.01 mole) of 2,6-dinitro-4-t-butylchlorobenzene was reacted with 3.1 grams of 40% aqueous solution of dimethylamine in 50 ml. ethanol. The temperature was slowly increased as follows: 30° C. for 1 hour, 40° C. for 1 hour, 50° C. for one hour, then 80° C. for five hours. When the reaction was complete, about 100 ml. H2O was added, precipitating the product. This was filtered, washed with portions of H2O and upon recrystallization from ethanol yielded 2.5 grams of N,N-dimethyl-2,6-dinitro-4-t-butylaniline in the form of orange-yellow needles melting at 101-102° C.

후처리

  1. temperatureThe temperature was slowly increased
  2. wait40° C. for 1 hour
  3. wait50° C. for one hour
  4. wait80° C. for five hours
  5. customprecipitating the product
  6. filtrationThis was filtered
  7. washwashed with portions of H2O and upon recrystallization from ethanol

출처 및 근거

ORD 기록
ord-3e70a35179374916b3a01ab5979ed78b
출처 데이터셋
uspto-grants-1978_03
특허 번호
US04077795

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