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

HRID 21730ノート

反応式

HRID 21730 の反応式
[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

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ecab1ddb575c4a79813f70eaa9956a8a
出典データセット
uspto-grants-1995_06
特許番号
US05424443

反応ノート

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