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1-Propanol → n-Propyl-4-chloro-3,5-dinitro-benzoate

HRID 1382129
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HRID 1382129 반응식
[CH2:1]([O:4][C:5](=[O:25])[C:6]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[C:9](N(CC=C)CC=C)=[C:8]([N+:22]([O-:24])=[O:23])[CH:7]=1)[CH2:2][CH3:3].[Cl:26]C1C([N+]([O-])=O)=CC(C(O)=O)=CC=1[N+]([O-])=O.C(O)CC>S(=O)(=O)(O)O.O>[CH2:1]([O:4][C:5](=[O:25])[C:6]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[C:9]([Cl:26])=[C:8]([N+:22]([O-:24])=[O:23])[CH:7]=1)[CH2:2][CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10311-PropanolHCID 83774-Chloro-3,5-dinitrobenzoic acidHCID 86742747n-Propyl-4-diallylamino-3,5-dinitro-benzoate

생성물 1

HCID 85970396n-Propyl-4-chloro-3,5-dinitro-benzoate

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매HCID 962Water
용매

실험 절차

According to a preferred form of realization of the process of the present invention n-propyl-4-diallylamino-3,5-dinitro-benzoate may be prepared by reacting 1 mole of 4-chloro-3,5-dinitro-benzoic acid with 1.25 moles of n-propanol at a temperature between 85° C. and 90° C., in the presence of a sulfuric acid catalyst, whereby the water formed is removed by azeotropic distillation with benzene. The distillation of water having been completed (5-7 hours) the reaction mixture, is cooled and the n-propyl-4-chloro-3,5-dinitro-benzoate is isolated. This compound is reacted with a 1.1 molar amount of diallyl amine at a temperature between 70° C. and 80° C., in an aqueous melt in the presence of 0.1 mole of 75% phosphoric acid and 1.05 moles of a 10% sodium hydroxide solution as acid binding agent. The reaction mixture is allowed to sedimentate, the organic phase is poured into water and the crystalline n-propyl-4-diallylamino-3,5-dinitro-benzoate is isolated.

후처리

  1. custommay be prepared
  2. customat a temperature between 85° C. and 90° C.
  3. customis removed by azeotropic distillation with benzene
  4. distillationThe distillation of water having
  5. custom(5-7 hours)
  6. temperatureis cooled

출처 및 근거

ORD 기록
ord-8371264fcf434420b4614a8e5c48ec21
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04806151

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