Ammonia → 2-Amino-3,6-difluorobenzonitrile

HRID 1418359ノート

反応式

HRID 1418359 の反応式
F[C:2]1[C:9]([F:10])=[CH:8][CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:5].O.[NH3:13]>C(#N)C>[NH2:13][C:2]1[C:9]([F:10])=[CH:8][CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:5]

参加物

5

反応物 3

HCID 222AmmoniaHCID 962WaterHCID 1456222,3,6-Trifluorobenzonitrile

生成物 1

HCID 450905912-Amino-3,6-difluorobenzonitrile

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

2,3,6-Trifluorobenzonitrile (1.76 ml, 15.2 mmol) in aqueous ammonia (20 ml) and acetonitrile (10 ml) was stirred for 7 days. Water was added. The whole was extracted with ether, the ether was dried (sodium sulphate) and evaporated. Flash column chromatography on silica gel, eluting with dichloromethane, gave the product (1.2 g), MS (+EI) 154 (M+), 1H NMR (CDCl3) 7.07-7.16 (1H, m), 6.36-6.43 (1H, m), 4.62 (2H, s).

後処理

  1. extractionThe whole was extracted with ether
  2. dry with materialthe ether was dried (sodium sulphate)
  3. customevaporated
  4. washFlash column chromatography on silica gel, eluting with dichloromethane

出典と根拠

ORDレコード
ord-d58cefe9ca844147a6bbb301c478e1e4
出典データセット
uspto-grants-1999_03
特許番号
US05883102

反応ノート

読み込み中…