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Water → 3-Chloro-6-hydrazino-2-methoxy-5-trifluoromethylpyridine

HRID 1871869
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HRID 1871869 반응식
O.[NH2:2][NH2:3].Cl[C:5]1[C:10]([C:11]([F:14])([F:13])[F:12])=[CH:9][C:8]([Cl:15])=[C:7]([O:16][CH3:17])[N:6]=1.O>C(O)CC>[Cl:15][C:8]1[C:7]([O:16][CH3:17])=[N:6][C:5]([NH:2][NH2:3])=[C:10]([C:11]([F:14])([F:13])[F:12])[CH:9]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 186895102,5-Dichloro-6-methoxy-3-trifluoromethylpyridine

생성물 1

HCID 186895243-Chloro-6-hydrazino-2-methoxy-5-trifluoromethylpyridine

시약·촉매·용매 1

HCID 10311-Propanol용매

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온도
90 °C

실험 절차

10.7 g (0.214 mol) of hydrazine hydrate were added in the course of 10 minutes with stirring at 50° C. to 25.0 g (0.102 mol) of 2,5-dichloro-6-methoxy-3-trifluoromethylpyridine in 100 ml of propanol and the mixture was stirred at 90° C. for 3 hours. After cooling, the resulting suspension was added to 1.2 liters of water, the precipitate was filtered off with suction and taken up in methylene chloride, and the solution was washed with water. The organic phase was dried and concentrated, and the residue was stirred with ether/pentane (1:1). After filtering off with suction and drying, 7.8 g (32% of theory) of the title compound of m.p. 140-142° C. were obtained.

후처리

  1. temperatureAfter cooling
  2. filtrationthe precipitate was filtered off with suction
  3. washthe solution was washed with water
  4. customThe organic phase was dried
  5. concentrationconcentrated
  6. stirringthe residue was stirred with ether/pentane (1:1)
  7. filtrationAfter filtering off with suction
  8. customdrying

출처 및 근거

ORD 기록
ord-2b6cebd1b92b48a297ebca162bf94059
출처 데이터셋
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06107253

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