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

HRID 510026노트

반응식

HRID 510026 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 were added to a suspension of 46.2 g (264.66 mmol) of 2-chloro-5-fluoronicotinamide in dichloromethane (783 ml), and the mixture was cooled to 0° C. Then, while stirring, 41.12 ml (291.13 mmol) of trifluoroacetic anhydride were slowly added dropwise and the mixture was stirred at 0° C. for 1.5 h. The reaction solution was subsequently washed twice with saturated aqueous sodium hydrogencarbonate solution (391 ml each time), dried and concentrated under reduced pressure.

후처리

  1. stirringthe mixture was stirred at 0° C. for 1.5 h
  2. washThe reaction solution was subsequently washed twice with saturated aqueous sodium hydrogencarbonate solution (391 ml each time)
  3. customdried
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1389f5bc688941218dd67aeb143edb2c
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096592B2

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