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3-Chloro-4-methoxyaniline → (3-Chloro-4-methoxyphenyl)hydrazine--hydrogen chloride (1/1)

HRID 429316
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HRID 429316 반응식
[N:1]([O-])=O.[Na+].[Cl:5][C:6]1[CH:7]=[C:8]([CH:10]=[CH:11][C:12]=1[O:13][CH3:14])[NH2:9]>O.Cl>[ClH:5].[Cl:5][C:6]1[CH:7]=[C:8]([NH:9][NH2:1])[CH:10]=[CH:11][C:12]=1[O:13][CH3:14]
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참가 물질

5

반응물 2

HCID 214413-Chloro-4-methoxyanilineHCID 23668193Sodium Nitrite

생성물 1

HCID 16495456(3-Chloro-4-methoxyphenyl)hydrazine--hydrogen chloride (1/1)수율 173.4%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매2회HCID 962Water용매

실험 절차

A solution of sodium nitrite (6 g) in water (50 ml) was added dropwise to a solution of 3-chloro-4-methoxyaniline (10 g) in concentrated hydrochloric acid (30 ml) at 0° C. with stirring. After the addition was completed, the reaction mixture was stirred at the same temperature for 1 hour. A solution of stannous chloride dihydrate (50 g) in concentrated hydrochloric acid (30 ml) was added dropwise at 0° C. The resulting mixture was stirred for 2 hours at the same temperature. The resulting precipitate was collected by filtration, washed with ice water and dried in vacuo at 50° C. to afford (3-chloro-4-methoxyphenyl)hydrazine hydrochloride (11.5 g) as a yellow brown solid.

후처리

  1. additionAfter the addition
  2. stirringthe reaction mixture was stirred at the same temperature for 1 hour
  3. stirringThe resulting mixture was stirred for 2 hours at the same temperature
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with ice water
  6. customdried in vacuo at 50° C.

출처 및 근거

ORD 기록
ord-f5cd6e83e0fe4815a4fc7f91dfbc66b6
출처 데이터셋
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06316485B1

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