1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) → HCID 178431852, 화합물

HRID 911923

반응식

HRID 911923 반응식
C1C=CC(C2C=CC=CC=2)=CC=1.C1C=CC(OC2C=CC=CC=2)=CC=1.CC1(C)O[C:31](=[O:33])[C:30](=[CH:34][NH:35][C:36]2[C:40]([CH3:41])=[CH:39][S:38][CH:37]=2)C(=O)O1>>[CH3:41][C:40]1[C:36]2=[N:35][CH:34]=[CH:30][C:31]([OH:33])=[C:37]2[S:38][CH:39]=1

참가 물질

3

반응물 2

HCID 246701,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene)HCID 669953662,2-Dimethyl-5-((4-methylthiophen-3-ylamino)methylene)-1,3-dioxane-4,6-dione

생성물 1

HCID 178431852HCID 178431852, 화합물수율 101.9%

반응 조건

온도
235 °C

실험 절차

A solution of Dowtherm A (7 mL) was heated in oil bath at 235° C. under nitrogen. 2,2-dimethyl-5-((4-methylthiophen-3-ylamino)methylene)-1,3-dioxane-4,6-dione (5.0 g, 19 mmol) was added in portions over a 20 minutes period. After the last portion was added, the solution stirred at 235° C. for another 5 minutes. The solution was removed from the oil bath and allowed to cool to room temperature. Upon cooling, the product precipitated out of solution. Diethyl ether was added and the solid was filtered and dried to give the title compound (3.2 g) with residual amounts of Dowtherm A remaining.

후처리

  1. additionAfter the last portion was added
  2. customThe solution was removed from the oil bath
  3. temperatureto cool to room temperature
  4. temperatureUpon cooling
  5. customthe product precipitated out of solution
  6. additionDiethyl ether was added
  7. filtrationthe solid was filtered
  8. customdried

출처 및 근거

ORD 기록
ord-539a958a87b240ed8fa6589d5c234605
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022223B2

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