M-Cresol → 2-(2-Hydroxy-4-methylphenyl)-4,6-bis(4-phenoxyphenyl)-1,3,5-triazine

HRID 23851

反応式

HRID 23851 の反応式
Cl[C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([O:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[CH:10][CH:9]=2)[N:5]=[C:4]([C:21]2[CH:26]=[CH:25][C:24]([O:27][C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)=[CH:23][CH:22]=2)[N:3]=1.[CH:34]1[C:39]([OH:40])=[CH:38][CH:37]=[CH:36][C:35]=1[CH3:41].[Al+3].[Cl-].[Cl-].[Cl-].N1C=CC=NN=1>ClC1C=CC=CC=1>[OH:40][C:39]1[CH:34]=[C:35]([CH3:41])[CH:36]=[CH:37][C:38]=1[C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][C:11]([O:14][C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[CH:10][CH:9]=2)[N:5]=[C:4]([C:21]2[CH:26]=[CH:25][C:24]([O:27][C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)=[CH:23][CH:22]=2)[N:3]=1

参加物

6

反応物 4

HCID 342M-CresolHCID 1230471,2,3-TriazineHCID 6451240Aluminum(III) ChlorideHCID 225686182-Chloro-4,6-bis(4-phenoxyphenyl)-1,3,5-triazine

生成物 1

HCID 1356219502-(2-Hydroxy-4-methylphenyl)-4,6-bis(4-phenoxyphenyl)-1,3,5-triazine

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

反応条件

温度
70 °C

実験手順

A mixture of 0.9 gm of 2-chloro-4,6-bis(4-phenoxyphenyl)-1,3,5-triazine, 0.24 gm of m-cresol and 0.4 gm AlCl3 in 5 ml chlorobenzene was heated to 70° C. under nitrogen and efficient stirring. After about 4 hr at 70° C., the reaction mixture was analyzed by HPLC, which showed the formation of a new product, and almost disappearance of the starting triazine. The reaction mixture was cooled to room temperature and quenched with water. It was then extracted with methylene chloride, and the organic layer separated, washed with water, dried, and concentrated to give a crude product. The crude product was crystallized from acetone to give almost pure 2-(2-hydroxy-4-methylphenyl)-4,6-bis(4-phenoxyphenyl)-1,3,5-triazine identified by HPLC, NMR and mass spectroscopy.

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customquenched with water
  3. extractionIt was then extracted with methylene chloride
  4. customthe organic layer separated
  5. washwashed with water
  6. customdried
  7. concentrationconcentrated
  8. customto give a crude product
  9. customThe crude product was crystallized from acetone

出典と根拠

ORDレコード
ord-3c8ad07ec9e243c7b04ad3605668233c
出典データセット
uspto-grants-2005_02
特許番号
US06855269B2

関連ノート

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