Sodium Hydroxide → 2-Chloro-p-Phenylenediamine

HRID 2082651

반응식

HRID 2082651 반응식
S(O)(O)(=O)=O.[Cl:6][C:7]1[CH:12]=[C:11]([NH2:13])[CH:10]=[CH:9][C:8]=1[NH2:14].[OH-].[Na+]>O>[Cl:6][C:7]1[CH:12]=[C:11]([NH2:13])[CH:10]=[CH:9][C:8]=1[NH2:14]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 225842-Chloro-p-phenylenediamine sulfate

생성물 1

HCID 119982-Chloro-p-Phenylenediamine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2-Chloro-1,4-phenylenediamine sulfate, ##STR9## was dissolved in water, neutralized with an aqueous sodium hydroxide solution, and extracted with ethyl ether. The ether extract layer, after removal of the ether, was purified by recrystallization, repeated twice, from chlorobenzene, and dried to obtain 2-chloro-1,4-phenylenediamine, ##STR10## In 500 ml of benzene, were dissolved 0.1 mole of said 2-chloro-1,4-phenylenediamine and 0.2 mole of distilled and dried p-methylbenzaldehyde. The resulting solution was refluxed for about 4 hours, while removing the azeotropically distilled water by means of a Dean-Stark trap. Thereafter, the solvent was removed from the reaction mixture by distillation by use of a rotary evaporator. The distillation residue was collected and purified by repeated recrystallization from isopropyl alcohol until a constant melting point was attained to obtain bis(4'-methylbenzal)-2-chloro-1,4-phenylenediamine, ##STR11## (Compound H), which showed M.R. of 144.4° - 196.6° C.

후처리

  1. extractionextracted with ethyl ether
  2. extractionThe ether extract layer
  3. customafter removal of the ether
  4. customwas purified by recrystallization
  5. customdried

출처 및 근거

ORD 기록
ord-59ba8f8ee0984b8cb746c7eadfa0ebf9
출처 데이터셋
uspto-grants-1978_04
특허 번호
US04082686

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