Ammonia → 2-Amino-3,6-difluorobenzonitrile

HRID 1418359노트

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HRID 1418359 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 450905912-Amino-3,6-difluorobenzonitrile

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d58cefe9ca844147a6bbb301c478e1e4
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05883102

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