Ammonium Hydroxide → HCID 178516142、化合物

HRID 1681199ノート

反応式

HRID 1681199 の反応式
[F:1][C:2]([F:16])([F:15])[C:3](=O)[CH2:4][C:5](=[O:13])[CH2:6][C:7]([C:9]([F:12])([F:11])[F:10])=O.[OH-].[NH4+:18]>>[F:1][C:2]([F:16])([F:15])[C:3]1[CH:4]=[C:5]([OH:13])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[N:18]=1

参加物

3

反応条件

温度
130 °C

実験手順

A mixture of 30 g 1,5-di(trifluoromethyl)-1,3,5-trioxopentane and 125 ml 28% aqueous ammonium hydroxide was heated in an autoclave at 130° C. for 5 hours. The reaction mixture was concentrated in vacuo, dissolved in 350 ml ethanol and treated with 11 ml 6N hydrochloric acid. The resulting mixture was concentrated in vacuo, 100 ml water added to the residue and filtered to give 8.0 g 2,6-di(trifluoromethyl)-4-hydroxypyridine, m.p. 123°-130° C.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutiondissolved in 350 ml ethanol
  3. additiontreated with 11 ml 6N hydrochloric acid
  4. concentrationThe resulting mixture was concentrated in vacuo, 100 ml water
  5. additionadded to the residue
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-dec5f2061bb746b79ca7ef18cd3eadc1
出典データセット
uspto-grants-1992_12
特許番号
US05169853

反応ノート

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