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Pyridine → N-Methyl-[5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-methylsulfinyl-1H-pyrazol-3-yl]ethanimine N-oxide

HRID 1738757
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HRID 1738757 반응식
[C:1]([C:4]1[C:8]([S:9]([CH3:11])=[O:10])=[C:7]([NH2:12])[N:6]([C:13]2[C:18]([Cl:19])=[CH:17][C:16]([C:20]([F:23])([F:22])[F:21])=[CH:15][C:14]=2[Cl:24])[N:5]=1)(=O)[CH3:2].Cl.[CH3:26][NH:27][OH:28].N1C=CC=CC=1>CO>[CH3:26][N+:27]([O-:28])=[C:1]([C:4]1[C:8]([S:9]([CH3:11])=[O:10])=[C:7]([NH2:12])[N:6]([C:13]2[C:18]([Cl:19])=[CH:17][C:16]([C:20]([F:23])([F:22])[F:21])=[CH:15][C:14]=2[Cl:24])[N:5]=1)[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 77906N-methylhydroxylamine hydrochlorideHCID 11069398Acetoprole

생성물 1

HCID 86754584N-Methyl-[5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-methylsulfinyl-1H-pyrazol-3-yl]ethanimine N-oxide수율 36.8%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
20 °C

실험 절차

A mixture of 2.0 grams (0.005 mole) of 3-acetyl-5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-methylsulfinyl-1H-pyrazole, 0.83 gram (0.01 mole) of N-methylhydroxylamine hydrochloride, 1.21 ml (0.015 mole) of pyridine and 150 ml of methanol was stirred 68 h at 20° C. The mixture was successively evaporated, washed with CH2Cl2 and water; filtered; washed in hot acetonitrile, acetone, hot methanol; and dried so as to give 0.79 gram of Compound No. 4 (m.p. about 228° C.).

후처리

  1. customThe mixture was successively evaporated
  2. washwashed with CH2Cl2 and water
  3. filtrationfiltered
  4. washwashed in hot acetonitrile
  5. customand dried so as

출처 및 근거

ORD 기록
ord-e10b30614fcd49fa99619dea30fc9dd8
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05965491

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