Sodium Hydroxide → 2-iodo-1,4-benzenediamine

HRID 1732867노트

반응식

HRID 1732867 반응식
[I:1][C:2]1[CH:8]=[C:7]([N+:9]([O-])=O)[CH:6]=[CH:5][C:3]=1[NH2:4].[OH-].[Na+]>Cl>[I:1][C:2]1[CH:8]=[C:7]([NH2:9])[CH:6]=[CH:5][C:3]=1[NH2:4]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 2226292-Iodo-4-nitroaniline

생성물 1

HCID 8191282-iodo-1,4-benzenediamine수율 20.9%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매2회

실험 절차

A mixture of concentrated hydrochloric acid (150 ml) and 2-iodo-4-nitroaniline (30.0 g) is stirred and warmed to 45°-50° C. A solution of stannous chloride dihydrate (90.0 g) in concentrated hydrochloric acid (110 ml) is added while maintaining the reaction temperature at 65°-70° C. After the addition is completed, the mixture is cooled in an ice bath and 50% sodium hydroxide (250 ml) is added slowly. The mixture is filtered and the isolated damp solid is stirred in 600 ml water at reflux. The solution is decolorized with charcoal, filtered and cooled to afford 5.55 g of title compound, m.p. 95°-99° C.

후처리

  1. temperaturewarmed to 45°-50° C
  2. temperaturewhile maintaining the reaction temperature at 65°-70° C
  3. additionAfter the addition
  4. temperaturethe mixture is cooled in an ice bath
  5. filtrationThe mixture is filtered
  6. stirringthe isolated damp solid is stirred in 600 ml water
  7. temperatureat reflux
  8. filtrationfiltered
  9. temperaturecooled

출처 및 근거

ORD 기록
ord-d6f0326b3a484b5ba354b692b59f8e97
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04239708

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