1,1'-Biphenyl, mixt. with 1,1'-oxybis(benzene) → HCID 178431852、化合物

HRID 335246ノート

反応式

HRID 335246 の反応式
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

参加物

3

反応物 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

生成物 1

HCID 178431852HCID 178431852、化合物収率 101.9%

反応条件

温度
235 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f3ca90f68ea342e08dd8ba26f047e9b2
出典データセット
uspto-grants-2014_11
特許番号
US08883828B2

反応ノート

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