Ammonia → 2-Amino-3-chloro-6-fluorobenzonitrile

HRID 1418361노트

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HRID 1418361 반응식
[NH3:1].[Cl:2][C:3]1[C:4](F)=[C:5]([C:8]([F:11])=[CH:9][CH:10]=1)[C:6]#[N:7]>C(#N)C>[NH2:1][C:4]1[C:3]([Cl:2])=[CH:10][CH:9]=[C:8]([F:11])[C:5]=1[C:6]#[N:7]

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 131752313-Chloro-2,6-difluorobenzonitrile

생성물 1

HCID 539633822-Amino-3-chloro-6-fluorobenzonitrile

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
60 °C

실험 절차

Aqueous ammonia (d 0.880, 2 ml) was added to a solution of 3-chloro-2,6-difluorobenzonitrile (1.93 g, 11.1 mmol) in acetonitrile (10 ml), and the mixture heated to 60° C. for 16 h. The resulting brown solution was evaporated and purified by flash chromatography eluting with 5% ethyl acetate/hexane, increasing the gradient to 20% ethyl acetate/hexane, to furnish a white solid (410 mg), MS (+EI) 173/171 (M+); 1H NMR (CDCl3) 7.39 (1H, dd, J5.7, 9.0 Hz), 6.46 (1H, t, J8.7 Hz), 4.95 (2H, br. s).

후처리

  1. customThe resulting brown solution was evaporated
  2. custompurified by flash chromatography
  3. washeluting with 5% ethyl acetate/hexane
  4. temperatureincreasing the gradient to 20% ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-d61ca91cb2c24af7af1640708fd82a99
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05883102

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