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Water → HCID 18689504, 화합물

HRID 1290142
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HRID 1290142 반응식
O.[NH2:2][NH2:3].[Cl:4][C:5]1[C:6](F)=[N:7][C:8]([F:15])=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1.O>C(O)CC>[Cl:4][C:5]1[C:6]([NH:2][NH2:3])=[N:7][C:8]([F:15])=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 11042190HCID 11042190, 화합물

생성물 1

HCID 18689504HCID 18689504, 화합물

시약·촉매·용매 1

HCID 10311-Propanol용매

실험 절차

10.5 g (0.21 mol) of hydrazine hydrate were added to a stirred mixture of 21.8 g (0.1 mol) of 3-chloro-2,6-difluoro-5-trifluoromethylpyridine in 100 ml of propanol at 50° C. in the course of 15 minutes, and stirring was continued for 2 hours at the same temperature. After cooling, the batch was poured into 1.5 l of water and the precipitate which had separated out was filtered off with suction. It was taken up in ethyl acetate for purification and extracted using water. After drying and concentration, 20.9 g (91% of theory) of the title compound of m.p. 104°-106° C. were obtained; a sublimated sample melted at 111°-113° C.

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후처리

  1. temperatureAfter cooling
  2. customthe precipitate which had separated out
  3. filtrationwas filtered off with suction
  4. customIt was taken up in ethyl acetate for purification
  5. extractionextracted
  6. customAfter drying
  7. concentrationconcentration, 20.9 g (91% of theory) of the title compound of m.p. 104°-106° C.
  8. customwere obtained

출처 및 근거

ORD 기록
ord-e7a7a7690e4b4f419f09e90d469d0d25
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05750705

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