Phenol → Phenol, 4,4'-[1,3-phenylenebis(1-methylethylidene)]bis-

HRID 429606

반응식

HRID 429606 반응식
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:8]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([C:17]([CH3:19])=[CH2:18])[CH:12]=1)([CH3:10])=[CH2:9]>CCCCCC>[CH3:18][C:17]([C:13]1[CH:14]=[CH:15][CH:16]=[C:11]([C:8]([C:4]2[CH:5]=[CH:6][C:1]([OH:7])=[CH:2][CH:3]=2)([CH3:10])[CH3:9])[CH:12]=1)([C:4]1[CH:5]=[CH:6][C:1]([OH:7])=[CH:2][CH:3]=1)[CH3:19]

참가 물질

4

반응물 2

HCID 996PhenolHCID 773531,3-Diisopropenylbenzene

생성물 1

HCID 3292100Phenol, 4,4'-[1,3-phenylenebis(1-methylethylidene)]bis-수율 22.3%

시약·촉매·용매 1

HCID 8058Hexane용매2회

반응 조건

온도
80 °C

실험 절차

A 500-ml three-neck reactor was charged with Amberlist-15 (7.5 g, 2.6 mmols), phenol (178.5 g, 633 mmols) and hexane (60 ml). The contents were heated up to 80° C in nitrogen atmosphere. Under agitation, a mixture of m-diisopropenylbenzene (m-DIPeB, 15.0 g, 31.5 mmols) and hexane (60 ml) was fed thereto over 3 hours at 80° C. After completion of the feed, agitation was carried out at 80° C. for 10 minutes and then Amberlist-15 was removed by filtration. The filtrate was analyzed by liquid chromatography. Bisphenol M (α, α″-bis(4-hydroxyphenyl)-1,3-diisopropylbenzene, 29.6 g, yield 90%), the intended product, and the o,p-product, the position isomer of bisphenol M (α-(4-hydroxyphenyl)-α″-(2-hydroxyphenyl)-1,3-diisopropylbenzene, 2.43 g, yield 7.4%), were obtained. After completion of the same aftertreatment and purification operations using p-xylene as those in Example 1, bisphenol M was isolated (22.0 g., isolation yield 67%, purity 99.5%).

후처리

  1. waitAfter completion of the feed, agitation was carried out at 80° C. for 10 minutes
  2. customAmberlist-15 was removed by filtration

출처 및 근거

ORD 기록
ord-db43bec801524535942cdcefdef6b9aa
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06316677B1

연결된 노트

불러오는 중…