Triethylamine → 4-Amino-3-fluorobenzonitrile

HRID 394795노트

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HRID 394795 반응식
CCOC(C)=O.[F:7][C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][C:16]=1[N+:17]([O-])=O)[C:11]([NH2:13])=O.CCN(CC)CC>C(Cl)Cl>[F:7][C:8]1[CH:9]=[C:10]([CH:14]=[CH:15][C:16]=1[NH2:17])[C:11]#[N:13]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 114239673-Fluoro-4-nitrobenzamide

생성물 1

HCID 27564314-Amino-3-fluorobenzonitrile수율 114.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a 0° C. EtOAc (150 mL) solution of 3-fluoro-4-nitrobenzamide (4.85 g, 26.4 mmol) and Et3N (5.34 g, 52.8 mmol) was added dropwise a CH2Cl2 (50 mL) solution of 1,1,1-trichloroacetyl chloride (5.28 g, 29.04 mmol). The reaction was complete in 2 h (TLC, 1:1 hexane:EtOAc), then it was washed with 1N HCl, dried (MgSO4) and evaporated to give 4.1 g of the corresponding nitrile.

후처리

  1. customTo a 0° C
  2. wash(TLC, 1:1 hexane:EtOAc), then it was washed with 1N HCl
  3. dry with materialdried (MgSO4)
  4. customevaporated

출처 및 근거

ORD 기록
ord-bb4c26d451f645b1a14d04531fcc5c55
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06602895B2

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