Potassium Carbonate → HCID 21938673, 화합물

HRID 382500노트

반응식

HRID 382500 반응식
I[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1.[Cl:9][C:10]1[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[C:11]=1[NH2:12].C(=O)([O-])[O-].[K+].[K+]>C1(C)C(C)=CC=CC=1.CCCCCCC.[Cu]>[Cl:9][C:10]1[CH:16]=[C:15]([F:17])[CH:14]=[C:13]([F:18])[C:11]=1[NH:12][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1

참가 물질

7

반응물 3

HCID 11430Potassium CarbonateHCID 122074-IodotolueneHCID 27340832-Chloro-4,6-difluoroaniline

생성물 1

HCID 21938673HCID 21938673, 화합물

시약·촉매·용매 3

HCID 23978Copper촉매HCID 7237O-Xylene용매HCID 8900Heptane용매

실험 절차

A mixture of 4-iodotoluene (210 g, 0.96 mol), 2-chloro-4,6-difluoroaniline (204 g, 1.25 mol), copper powder (36 g, 0.57 mol), cuprous iodide (130 g, 0.68 mol), and potassium carbonate (118 g, 0.86 mol) in 500 ml of xylene is stirred vigorously and heated to reflux in a flask fitted with a Dean-Stark trap for 26 hours. After cooling to room temperature, the solids are filtered off, and the filter cake is washed with 100 ml of xylene. The solvents are evaporated under reduced pressure to give an oil which is dissolved in a mixture of 50 g of silica gel in 750 ml of heptane. The solids are filtered off and the solvents are evaporated under reduced pressure to give N-(2′-chloro-4′,6′-difluorophenyl)-4-methylaniline as an oil.

후처리

  1. temperatureheated
  2. temperatureto reflux in a flask
  3. customfitted with a Dean-Stark trap for 26 hours
  4. filtrationthe solids are filtered off
  5. washthe filter cake is washed with 100 ml of xylene
  6. customThe solvents are evaporated under reduced pressure
  7. customto give an oil which
  8. filtrationThe solids are filtered off
  9. customthe solvents are evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-f36873b89aac4a73bec3ecf9ab6dd02d
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06310099B1

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