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Ammonium Chloride → HCID 18005445, 화합물

HRID 989241
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HRID 989241 반응식
[H-].[K+].[NH2:3][C:4]1[N:8]([C:9]2[C:14]([Cl:15])=[CH:13][C:12]([C:16]([F:19])([F:18])[F:17])=[CH:11][C:10]=2[Cl:20])[N:7]=[C:6]([C:21]#[N:22])[C:5]=1[S:23]([CH3:25])=[O:24].[CH2:26]([S:28]([CH:31]=[CH2:32])(=[O:30])=[O:29])[CH3:27].[Cl-].[NH4+]>CN(C)C=O>[Cl:20][C:10]1[CH:11]=[C:12]([C:16]([F:17])([F:18])[F:19])[CH:13]=[C:14]([Cl:15])[C:9]=1[N:8]1[C:4]([NH:3][CH2:27][CH2:26][S:28]([CH2:31][CH3:32])(=[O:30])=[O:29])=[C:5]([S:23]([CH3:25])=[O:24])[C:6]([C:21]#[N:22])=[N:7]1
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6

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HCID 25517Ammonium ChlorideHCID 74680(Ethylsulfonyl)etheneHCID 82127Potassium hydrideHCID 108618955-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-methylsulfinylpyrazole

생성물 1

HCID 18005445HCID 18005445, 화합물수율 31.1%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매
3회

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온도
20 °C

실험 절차

To a suspension of 35% potassium hydride in oil (0.7 g) in dry N,N-dimethylformamide (DMF) was added a solution of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-(methylsulfinyl)-1H-pyrazole-3-carbonitrile (10.0 g) in dry DMF dropwise at 4° C. over 10 minutes. After stirring for 20 minutes, vinyl ethyl sulfone (3.13 g) in dry DMF was added during 5 hours at 4° C. The mixture was stirred overnight under nitrogen with warming to 20° C. Ammonium chloride was added at 4° C., and the mixture extracted (ethyl acetate), washed twice with water, dried (sodium sulfate) and evaporated. Crystallization from ethyl acetate/methanol/hexane gave 1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-5-[2-(ethylsulfonyl)ethylamino]-4-(methylsulfinyl)-1H-pyrazole-3-carbonitrile (4.08 g), m.p.131-132° C. By proceeding in a similar manner the following compounds were prepared:

후처리

  1. stirringThe mixture was stirred overnight under nitrogen
  2. extractionthe mixture extracted (ethyl acetate)
  3. washwashed twice with water
  4. dry with materialdried (sodium sulfate)
  5. customevaporated
  6. customCrystallization from ethyl acetate/methanol/hexane

출처 및 근거

ORD 기록
ord-0adbf66a133a438da1bde4a173119796
출처 데이터셋
uspto-grants-2003_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06638956B2

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