Triethylamine → 2-Chloro-5-fluoropyridine-3-carbonitrile

HRID 536476노트

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HRID 536476 반응식
C(N(CC)CC)C.[Cl:8][C:9]1[N:17]=[CH:16][C:15]([F:18])=[CH:14][C:10]=1[C:11]([NH2:13])=O.FC(F)(F)C(OC(=O)C(F)(F)F)=O>ClCCl>[Cl:8][C:9]1[N:17]=[CH:16][C:15]([F:18])=[CH:14][C:10]=1[C:11]#[N:13]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 9845Trifluoroacetic anhydrideHCID 126297962-Chloro-5-fluoropyridine-3-carboxamide

생성물 1

HCID 231108512-Chloro-5-fluoropyridine-3-carbonitrile

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

81.2 ml (582.25 mmol) of triethylamine was added to a suspension of 46.2 g (264.66 mmol) of 2-chloro-5-fluoronicotinamide in dichloromethane (783 ml) and cooled to 0° C. While stirring, 41.12 ml (291.13 mmol) of trifluoroacetic acid anhydride was slowly added dropwise and stirred for a further 1.5 h at 0° C. The reaction solution was then washed twice with saturated aqueous sodium hydrogen carbonate solution (391 ml each time), dried and concentrated by vacuum evaporation.

후처리

  1. stirringstirred for a further 1.5 h at 0° C
  2. washThe reaction solution was then washed twice with saturated aqueous sodium hydrogen carbonate solution (391 ml each time)
  3. customdried
  4. concentrationconcentrated by vacuum evaporation

출처 및 근거

ORD 기록
ord-9f1ee4999b1e41029805d4fc7eb963d2
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859569B2

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