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

HRID 1418361ノート

反応式

HRID 1418361 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d61ca91cb2c24af7af1640708fd82a99
出典データセット
uspto-grants-1999_03
特許番号
US05883102

反応ノート

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