Sodium disulfide → 3-(3-Phenyl-1-propenyl)aniline

HRID 1903651

반응식

HRID 1903651 반응식
[C:1]1([CH2:7][CH:8]=[CH:9][C:10]2[CH:11]=[C:12]([N+:16]([O-])=O)[CH:13]=[CH:14][CH:15]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.N.[S-][S-].[Na+].[Na+]>C(O)C>[C:1]1([CH2:7][CH:8]=[CH:9][C:10]2[CH:11]=[C:12]([CH:13]=[CH:14][CH:15]=2)[NH2:16])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 89870Sodium disulfideHCID 12896473Azane;hydrateHCID 538829723-(3-Phenyl-1-propenyl)nitrobenzene

생성물 1

HCID 540429893-(3-Phenyl-1-propenyl)aniline수율 85%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 3-(3-phenyl-1-propenyl)nitrobenzene (10.5 g) in 200 ml of ethanol were added 70 ml of 35% ammonia water and 44 g of sodium disulfide. After heating under reflux for 2 hours, the solvent was removed under reduced pressure, followed by extraction with ethyl acetate. The extract was washed with water and dried over magnesium sulfate. The solvent was removed by distillation under reduced pressure to give 7.8 g of 3-(3-phenyl-1-propenyl)aniline (yield, 85%). B.P. 128°-130° C./0.09 mmHg.

후처리

  1. temperatureAfter heating
  2. temperatureunder reflux for 2 hours
  3. customthe solvent was removed under reduced pressure
  4. extractionfollowed by extraction with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was removed by distillation under reduced pressure

출처 및 근거

ORD 기록
ord-0fca6851e60a46b480237d921ebc77b7
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04437880

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