Hydrochloric Acid → 2-(2,4-Dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine

HRID 1066444

反応式

HRID 1066444 の反応式
[C:1]1([C:7]2[N:12]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[N:10]=[C:9](Cl)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[C:21]1([CH:28]=[CH:27][CH:26]=[C:24]([OH:25])[CH:23]=1)[OH:22].C[O-].[Na+]>C1S(=O)(=O)CCC1.CO.C1(C)C(C)=CC=CC=1>[C:1]1([C:7]2[N:12]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[N:10]=[C:9]([C:26]3[CH:27]=[CH:28][C:21]([OH:22])=[CH:23][C:24]=3[OH:25])[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 5054ResorcinolHCID 196982-Chloro-4,6-diphenyl-1,3,5-triazineHCID 10942334Sodium Methoxide

生成物 1

HCID 1354371252-(2,4-Dihydroxyphenyl)-4,6-diphenyl-1,3,5-triazine

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 7237O-Xylene溶媒HCID 31347Sulfolane溶媒

反応条件

温度
118 °C

実験手順

A 500 mL three-necked, round-bottomed flask equipped with a mechanical stirrer is charged with 60 g of xylene and 55.5 g (0.207) of 4,6-diphenyl-2-chloro-s-triazine. The mixture is warmed to 118° C. and the pressure is reduced to 300 mbar and 2.8 g of hydrogen chloride gas is charged to the system. The mixture is cooled to 80° C. and a solution of resorcinol (88.2 g, 0.802 mol) in 60 g of tetramethylene sulfone is added dropwise over a 7-minute period. The mixture is stirred at 80° C. for six hours and then for one hour at 100° C. The temperature is reduced to 60° C. and a 300 mL portion of methanol is added. The mixture is allowed to cool to room temperature and is stirred overnight. Sodium methoxide (41.3 g) is added portionwise to adjust the pH to 5.0-5.5. The solids are collected by vacuum filtration and are washed with methanol and water. After drying, the title compound is obtained in a yield of 59.2 g as a pale yellow solid.

後処理

  1. customA 500 mL three-necked, round-bottomed flask equipped with a mechanical stirrer
  2. additionis charged to the system
  3. temperatureThe mixture is cooled to 80° C.
  4. waitfor one hour at 100° C
  5. customis reduced to 60° C.
  6. temperatureto cool to room temperature
  7. stirringis stirred overnight
  8. filtrationThe solids are collected by vacuum filtration
  9. washare washed with methanol and water
  10. customAfter drying

出典と根拠

ORDレコード
ord-b4fb05a14f424cdcbcd193bd5795b8a8
出典データセット
uspto-grants-2001_06
特許番号
US06242598B1

関連ノート

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