Hydrochloric Acid → HCID 23358997, 화합물

HRID 232664노트

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HRID 232664 반응식
S(=O)(=O)(O)O.N([O-])=O.[Na+].[F:10][C:11]1[C:17]([F:18])=[C:16]([CH3:19])[C:15]([F:20])=[CH:14][C:12]=1N.[ClH:21]>C(O)(=O)C.[Cu]Cl>[F:18][C:17]1[C:11]([F:10])=[C:12]([Cl:21])[CH:14]=[C:15]([F:20])[C:16]=1[CH3:19]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 1118Sulfuric AcidHCID 184250192,3,5-Trifluoro-4-methylanilineHCID 23668193Sodium Nitrite

생성물 1

HCID 23358997HCID 23358997, 화합물

시약·촉매·용매 2

HCID 62652Cuprous chloride촉매HCID 176Acetic Acid용매

반응 조건

온도
70 °C

실험 절차

To conc. sulfuric acid (3 ml) is added sodium nitrite (0.3 g). The mixture is stirred at 70° C. for 10 minutes and then cooled to below 40° C. and thereto a solution of 2,3,5-trifluoro-4-methylaniline (0.48 g) in acetic acid (5 ml) is added dropwise below 40° C. After stirring for 30 minutes, the reaction mixture is added dropwise to a solution of copper (I) chloride (1.04 g) in conc. hydrochloric acid (10.4 ml) and the mixture is stirred at 80° C. for 30 minutes and then cooled. The resultant mixture is poured into ice-water, extracted with dichloromethane, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and purified by silica-gel column-chromatography (eluent; dichloromethane: n-hexane=1:4) to give 2,3,6-trifluoro-4-chlorotoluene (0.22 g).

후처리

  1. temperaturecooled to below 40° C.
  2. stirringAfter stirring for 30 minutes
  3. stirringthe mixture is stirred at 80° C. for 30 minutes
  4. temperaturecooled
  5. extractionextracted with dichloromethane
  6. washthe extract is washed with water
  7. customdried
  8. distillationThe solvent is distilled off under reduced pressure
  9. custompurified by silica-gel column-chromatography (eluent; dichloromethane: n-hexane=1:4)

출처 및 근거

ORD 기록
ord-9eea9288c44845239e59941f5d1a9cf0
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591744

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