4-Fluoro-3-methylbenzamide → 4-Fluoro-3-methylbenzonitrile

HRID 551171ノート

反応式

HRID 551171 の反応式
[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=O)=[CH:4][C:3]=1[CH3:11]>P(Cl)(Cl)(Cl)=O>[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]#[N:8])=[CH:4][C:3]=1[CH3:11]

参加物

3

反応物 1

HCID 27745784-Fluoro-3-methylbenzamide

生成物 1

HCID 27791804-Fluoro-3-methylbenzonitrile

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

10.00 g (65.29 mmol) 4-fluoro-3-methyl-benzoic acid amide are stirred together with 50 ml phosphorus oxychloride for 4 hours at 60° C. and then evaporated down i. vac. The residue is poured into ice water, the resulting precipitate is filtered off and washed with water. After being taken up in ethyl acetate the organic phase is washed with sat. potassium carbonate solution, dried over sodium sulphate and evaporated down completely i. vac.

後処理

  1. customevaporated down i
  2. additionThe residue is poured into ice water
  3. filtrationthe resulting precipitate is filtered off
  4. washwashed with water
  5. washis washed with sat. potassium carbonate solution
  6. dry with materialdried over sodium sulphate
  7. customevaporated down completely i

出典と根拠

ORDレコード
ord-963c69b4eb6849548cd8ca0fff2a7699
出典データセット
uspto-grants-2011_05
特許番号
US07947700B2

反応ノート

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