Hydrochloric Acid → 2-(5-Chloro-2,4-dihydroxyphenyl)-4,6-diphenyl-s-triazine

HRID 265827

반응식

HRID 265827 반응식
Cl[C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:3]=1.[Cl-].[Al+3].[Cl-].[Cl-].[Cl:24][C:25]1[CH:31]=[CH:30][C:28]([OH:29])=[CH:27][C:26]=1[OH:32].Cl>C1(C)C(C)=CC=CC=1>[Cl:24][C:25]1[C:26]([OH:32])=[CH:27][C:28]([OH:29])=[C:30]([C:2]2[N:7]=[C:6]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[N:5]=[C:4]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[N:3]=2)[CH:31]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 17314-ChlororesorcinolHCID 196982-Chloro-4,6-diphenyl-1,3,5-triazineHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 1358435932-(5-Chloro-2,4-dihydroxyphenyl)-4,6-diphenyl-s-triazine

시약·촉매·용매 1

HCID 7237O-Xylene용매

반응 조건

온도
80 °C

실험 절차

To a 350 mL sulfonation flask equipped with a mechanical stirrer, condenser and a nitrogen atmosphere are charged 26.8 g (100 mmol) of 2-chloro-4,6-diphenyl-s-triazine, and 100 mL of xylene (mixture of isomers). To the beige suspension are added 14.9 g (112 mmol) of aluminum chloride in one portion. The mixture is warmed to ca. 80° C. for 2 hours. 17.4 g (120 mmol) of 4-chlororesorcinol are then added in five portions over 40 minutes to the now homogeneous solution. The reaction mixture is heated at 90° C. for 42 hours and refluxed for another 24 hours. After cooling to room temperature, the contents of the flask are poured into 100 mL of 12% aqueous hydrochloric acid. The precipitate formed is removed by filtration, washed to pH 7 with water, rinsed with methanol and dried at 70° C. under vacuum. The title compound is obtained as a crude ocher-red product (29.5 g) and melts at 255°-265° C. It can be used without further purification.

후처리

  1. customTo a 350 mL sulfonation flask equipped with a mechanical stirrer, condenser
  2. temperatureThe reaction mixture is heated at 90° C. for 42 hours
  3. temperaturerefluxed for another 24 hours
  4. temperatureAfter cooling to room temperature
  5. customThe precipitate formed
  6. customis removed by filtration
  7. washwashed to pH 7 with water
  8. washrinsed with methanol
  9. customdried at 70° C. under vacuum

출처 및 근거

ORD 기록
ord-07c22cf583b04b7396cdc31ed18646ef
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05648488

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