Hydrochloric Acid → N-(1-ethylpropyl)-3,4-dimethylaniline

HRID 2163624

反応式

HRID 2163624 の反応式
[N+]([C:4]1[C:15]([CH3:16])=[C:14]([CH3:17])[CH:13]=[C:12]([N+]([O-])=O)[C:5]=1[NH:6][CH:7]([CH2:10][CH3:11])[CH2:8][CH3:9])([O-])=O.[N+](C1C(C)=C(C)C=C([N+]([O-])=O)C=1N(N=O)C(CC)CC)([O-])=O.S(=O)(=O)(O)N.Cl>O.C(Cl)CCl>[CH2:8]([CH:7]([NH:6][C:5]1[CH:12]=[CH:13][C:14]([CH3:17])=[C:15]([CH3:16])[CH:4]=1)[CH2:10][CH3:11])[CH3:9]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 5987Sulfamic AcidHCID 38479PendimethalinHCID 50260Nitroso-pendimethalin

生成物 1

HCID 91984N-(1-ethylpropyl)-3,4-dimethylaniline

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To a crude nitration solution comprising 1550 g. of 2,6-dinitro-N-(1-ethylpropyl)-3,4-dimethylaniline and 340 g. of 2,6-dinitro-N-nitroso-N-(1-ethylpropyl)-3,4-dimethylaniline in 3700 mls. of ethylene dichloride was added 212 g. of sulfamic acid and 2850 mls. of 37.7% hydrochloric acid. The mixture was refluxed at 80° C. for six hours, 2-liters of water was added thereto and the aqueous phase was separated. The aqueous phase was extracted with 500 ml. of ethylene dichloride and the organic phases were combined. The combined organic phase was washed with 3-liters of water, the aqueous phase separated and the ethylene dichloride was removed under vacuum at 68° C. to recover 1915 g. of product containing 1820 g. of 2,6-dinitro-N-(1-ethylpropyl)-3,4-dimethylaniline and less than 0.1% of 2,6-dinitro-N-nitroso-N-(1-ethylpropyl)-3,4-dimethylaniline.

後処理

  1. customthe aqueous phase was separated
  2. extractionThe aqueous phase was extracted with 500 ml
  3. washThe combined organic phase was washed with 3-liters of water
  4. customthe aqueous phase separated
  5. customthe ethylene dichloride was removed under vacuum at 68° C.
  6. customto recover 1915 g
  7. additionof product containing 1820 g

出典と根拠

ORDレコード
ord-f3b71956e65b4282bb8923768fe552de
出典データセット
uspto-grants-1979_01
特許番号
US04136117

関連ノート

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