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Phenyl 4-methylbenzoate → HCID 53937160、化合物

HRID 231658
ノート
印刷プレビュー

反応式

HRID 231658 の反応式
[C:1]1([CH3:16])[CH:6]=[CH:5][C:4]([C:7]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:8])=[CH:3][CH:2]=1.[S]>CC(C)=O>[C:1]1([CH:16]=[CH:16][C:1]2[CH:2]=[CH:3][C:4]([C:7]([O:9][C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=3)=[O:8])=[CH:5][CH:6]=2)[CH:6]=[CH:5][C:4]([C:7]([O:9][C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[O:8])=[CH:3][CH:2]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 219444Phenyl 4-methylbenzoate2 回HCID 5362487Sulfur

生成物 1

HCID 53937160HCID 53937160、化合物収率 5.9%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

反応条件

温度
80 °C

実験手順

Sixty five g (0.306 mole) of neat phenyl p-toluate were maintained in the temperature range of 280°-310° C. (boiling point) while a slow stream of nitrogen was bubbled in from below the surface (sparged). Sulfur (1.92 g, 0.060 mole) dissolved in more phenyl p-toluate (20 g, 0.099 mole) at 100° C. was added slowly with stirring over a period of 2-3 hours. The heating, stirring and nitrogen sparging were continued an additional four hour and then the mixture was allowed to cool near 80° C. and 100 mL of boiling acetone was added. The suspension was transferred to a larger flask and an additional 400 mL of acetone was added. The suspension was filtered at the boil to yield 3.8 g of diphenyl 4,4'-stilbenedicarboxylate.

後処理

  1. customwas bubbled in from below the surface (sparged)
  2. additionwas added slowly
  3. stirringThe heating, stirring
  4. waitnitrogen sparging were continued an additional four hour
  5. customThe suspension was transferred to a larger flask
  6. filtrationThe suspension was filtered at the boil

出典と根拠

ORDレコード
ord-3782f297a890490c9aa70b8bb2de398e
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04847407

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート