Dimethylformamide → 7-(alpha,alpha,alpha-Trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine-3-carboxaldehyde

HRID 225298

反応式

HRID 225298 の反応式
[P].[F:2][C:3]([F:20])([F:19])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]2[N:15]3[N:16]=[CH:17][CH:18]=[C:14]3[N:13]=[CH:12][CH:11]=2)[CH:5]=1.[OH-].[Na+].CN(C)[CH:25]=[O:26]>>[F:20][C:3]([F:19])([F:2])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([C:10]2[N:15]3[N:16]=[CH:17][C:18]([CH:25]=[O:26])=[C:14]3[N:13]=[CH:12][CH:11]=2)[CH:5]=1

参加物

5

実験手順

Seventy-five milliliters of dried dimethylformamide is cooled in an ice bath and 25 ml. of phosphorus osychloride is added dropwise with swirling. To this ice cold mixture is added 19.5 g. of 7-(α,α,α-trifluoro-m-tolyl)pyrazolo[1,5-a]pyrimidine in one portion and the reaction mixture is then heated on a steam bath for 1.5 hours. The mixture is poured onto ice and made basic (pH 10) with 10 N NaOH. The precipitated solid is removed by filtration and recrystallized from methylene chloride-hexane to give the product, m.p. 196°-198° C.

後処理

  1. additionThe mixture is poured onto ice
  2. customThe precipitated solid is removed by filtration
  3. customrecrystallized from methylene chloride-hexane
  4. customto give the product, m.p. 196°-198° C.

出典と根拠

ORDレコード
ord-efe35094456244b4878fa9c8652b6426
出典データセット
uspto-grants-1980_11
特許番号
US04236005

関連ノート

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