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

HRID 1678834ノート

反応式

HRID 1678834 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3e70a35179374916b3a01ab5979ed78b
出典データセット
uspto-grants-1978_03
特許番号
US04077795

反応ノート

読み込み中…