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Acetic Anhydride → HCID 20453877, 화합물

HRID 1462136
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HRID 1462136 반응식
[NH2:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:16])[F:15])=[C:9]([Cl:18])[C:8]=2[Cl:19])[N:5]=[CH:4][C:3]=1[C:20]#[N:21].[C:22](OC(=O)C)(=[O:24])[CH3:23]>O>[C:22]([NH:1][C:2]1[N:6]([C:7]2[C:12]([Cl:13])=[CH:11][C:10]([C:14]([F:17])([F:15])[F:16])=[C:9]([Cl:18])[C:8]=2[Cl:19])[N:5]=[CH:4][C:3]=1[C:20]#[N:21])(=[O:24])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 13122001HCID 13122001, 화합물

생성물 1

HCID 20453877HCID 20453877, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

5-Amino-4-cyano-1-(2,3,6-trichloro-4-trifluoromethylphenyl)pyrazole (3.74 g) in acetic anhydride (20 ml) was heated at reflux for 6 hours. The reaction mixture was then evaporated under reduced pressure to remove unreacted acetic anhydride. The residual oil was dissolved in dichloromethane (50 ml) and filtered. The filtrate was evaporated to give a foam, which was then suspended in water (70 ml). The suspension was filtered and the filtrate deposited a solid on standing. The solid was collected by filtration and washed with water to give 5-acetamido-4-cyano-1-(2,3,6-trichloro-4-trifluoromethylphenyl)pyrazole (0.4 g), m.p. 177°-178° C., in the form of a fawn-coloured solid.

후처리

  1. temperatureat reflux for 6 hours
  2. customThe reaction mixture was then evaporated under reduced pressure
  3. customto remove unreacted acetic anhydride
  4. dissolutionThe residual oil was dissolved in dichloromethane (50 ml)
  5. filtrationfiltered
  6. customThe filtrate was evaporated
  7. customto give a foam, which
  8. filtrationThe suspension was filtered
  9. filtrationThe solid was collected by filtration
  10. washwashed with water

출처 및 근거

ORD 기록
ord-0fbe4585ccd74e27bdad730164787c32
출처 데이터셋
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04459150

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