Sodium Hydroxide → 2-Methoxymethylphenylhydrazine

HRID 916731

반응식

HRID 916731 반응식
[CH3:1][O:2][CH2:3][C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH2:6].[N:11]([O-])=O.[Na+].[OH-].[Na+]>Cl.O>[CH3:1][O:2][CH2:3][C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH:6][NH2:11]

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 123343062-(Methoxymethyl)anilineHCID 23668193Sodium Nitrite

생성물 1

HCID 129793652-Methoxymethylphenylhydrazine수율 71%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매2회HCID 962Water용매

반응 조건

온도
-10 °C

실험 절차

6.86 g (50 m moles) of 2-methoxymethylaniline was dissolved in 50 ml of concentrated hydrochloric acid. The solution was cooled to −10° C. Thereto was dropwise added a solution of sodium nitrite (4.14 g, 60 m moles) dissolved in water (50 ml) while a temperature of −10° C. to 0° C. was being kept. Then, a solution of 44.6 g (235 m moles) of stannous chloride dissolved in concentrated hydrochloric acid (50 ml) was dropwise added at the above temperature in 1 hour. After the completion of the dropwise addition, stirring was conducted with a gradual temperature increase to about 20° C. Then, a 10% aqueous sodium hydroxide solution was dropped to obtain a pH of 14, after which extraction with toluene was conducted. The toluene layer was washed with water and concentrated under reduced pressure using a rotary evaporator to obtain 5.40 g (35.5 m moles) of liquid 2-methoxymethylphenylhydrazine. Yield: 71%.

후처리

  1. additionwas dropwise added at the above temperature in 1 hour
  2. additionAfter the completion of the dropwise addition
  3. temperatureincrease to about 20° C
  4. customto obtain a pH of 14
  5. extractionafter which extraction with toluene
  6. washThe toluene layer was washed with water
  7. concentrationconcentrated under reduced pressure
  8. customa rotary evaporator

출처 및 근거

ORD 기록
ord-bff5a41a01c241e79c1ed5d9deae2027
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07271263B2

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