Phosphorus oxychloride → 3-Chloro-2-(2,4-dichloro-6-fluorobenzothiazol-7-yl)-4,5,6,7-tetrahydro-2H-indazole

HRID 21730노트

반응식

HRID 21730 반응식
[Cl:1][C:2]1[S:3][C:4]2[C:10]([N:11]3[C:19](=O)[C:18]4[CH2:17][CH2:16][CH2:15][CH2:14][C:13]=4[NH:12]3)=[C:9]([F:21])[CH:8]=[C:7]([Cl:22])[C:5]=2[N:6]=1.P(Cl)(Cl)([Cl:25])=O>>[Cl:25][C:19]1[N:11]([C:10]2[C:4]3[S:3][C:2]([Cl:1])=[N:6][C:5]=3[C:7]([Cl:22])=[CH:8][C:9]=2[F:21])[N:12]=[C:13]2[C:18]=1[CH2:17][CH2:16][CH2:15][CH2:14]2

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 199334592-(2,4-Dichloro-6-fluorobenzothiazol-7-yl)1,3,4,5,6,7-hexahydro-2H-indazol-3-one

생성물 1

HCID 199334603-Chloro-2-(2,4-dichloro-6-fluorobenzothiazol-7-yl)-4,5,6,7-tetrahydro-2H-indazole

실험 절차

0.2 g 2-(2,4-Dichloro-6-fluorobenzothiazol-7-yl)1,3,4,5,6,7-hexahydro-2H-indazol-3-one was treated with 2 ml phosphorus oxychloride and the mixture stirred for one hour under reflux. After cooling, it was poured into ice-water, extracted with ethyl acetate and the organic phase washed with sodium hydrogen carbonate and water. It was dried over magnesium sulfate and concentrated. The residue was purified by column chromatography. Yield: 0.07 g=32% of theory m.p.: 161°-163° C.

후처리

  1. temperatureunder reflux
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. washthe organic phase washed with sodium hydrogen carbonate and water
  5. dry with materialIt was dried over magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-ecab1ddb575c4a79813f70eaa9956a8a
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05424443

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