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Phenyl 4-methylbenzoate → HCID 53937160, 화합물

HRID 414130
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HRID 414130 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 219444Phenyl 4-methylbenzoate2회HCID 5362487Sulfur

생성물 1

HCID 53937160HCID 53937160, 화합물수율 5.9%

시약·촉매·용매 1

HCID 180Acetone용매2회

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온도
80 °C

실험 절차

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 hours 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.

후처리

  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 hours
  5. customThe suspension was transferred to a larger flask
  6. filtrationThe suspension was filtered at the boil

출처 및 근거

ORD 기록
ord-a85bce63d1264a2a8a5f823f0485c051
출처 데이터셋
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04789755

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