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

HRID 551171노트

반응식

HRID 551171 반응식
[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]

참가 물질

3

반응물 1

HCID 27745784-Fluoro-3-methylbenzamide

생성물 1

HCID 27791804-Fluoro-3-methylbenzonitrile

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-963c69b4eb6849548cd8ca0fff2a7699
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947700B2

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