Hydrochloric Acid → 2-(2,4-Dihydroxy-5-hexylphenyl)-4,6-diphenyl-s-triazine

HRID 265826

反応式

HRID 265826 の反応式
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-].[CH2:24]([C:30]1[CH:36]=[CH:35][C:33]([OH:34])=[CH:32][C:31]=1[OH:37])[CH2:25][CH2:26][CH2:27][CH2:28][CH3:29].Cl>C1(C)C(C)=CC=CC=1>[OH:34][C:33]1[CH:32]=[C:31]([OH:37])[C:30]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[CH:36][C:35]=1[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

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 3610HexylresorcinolHCID 196982-Chloro-4,6-diphenyl-1,3,5-triazineHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 1358435832-(2,4-Dihydroxy-5-hexylphenyl)-4,6-diphenyl-s-triazine

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
80 °C

実験手順

To a 350 mL sulfonation flask equipped with a mechanical stirrer, condenser and a nitrogen atmosphere are charged 21.4 g (80 mmol) of 2-chloro-4,6-diphenyl-s-triazine, and 100 mL of xylene (mixture of isomers). To the beige suspension are added 11.3 g (85 mmol) of aluminum chloride in one portion. The mixture is warmed to ca. 80° C. for 45 minutes. 18.8 g (96 mmol) of 4-hexylresorcinol are then added in five portions over 40 minutes to the now homogeneous solution. The reaction mixture is heated at 90° C. for 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 orange product (29.2 g) and melts at 209°-213° C. It can be used without further purification.

後処理

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

出典と根拠

ORDレコード
ord-be2ac3c861e849cbb268cdf74a8d6947
出典データセット
uspto-grants-1997_07
特許番号
US05648488

関連ノート

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