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

HRID 2163624

반응식

HRID 2163624 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f3b71956e65b4282bb8923768fe552de
출처 데이터셋
uspto-grants-1979_01
특허 번호
US04136117

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