Toluene → N,N-bis[3-(2-ethoxycarbonylethyl)phenyl]-3,4-xylidine

HRID 3023

反応式

HRID 3023 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[C:4]([CH3:9])[CH:3]=1.I[C:11]1[CH:12]=[C:13]([CH:21]=[CH:22][CH:23]=1)[CH2:14][CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17].[C:24](=[O:27])([O-])[O-:25].[K+].[K+].CCCCC[CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42].[C:43]1(C)C=CC=C[CH:44]=1>O.O.O.O.O.S([O-])([O-])(=O)=O.[Cu+2]>[CH2:19]([O:18][C:16]([CH2:15][CH2:14][C:13]1[CH:12]=[C:11]([N:1]([C:41]2[CH:40]=[CH:39][CH:38]=[C:37]([CH2:36][CH2:35][C:24]([O:25][CH2:43][CH3:44])=[O:27])[CH:42]=2)[C:2]2[CH:7]=[CH:6][C:5]([CH3:8])=[C:4]([CH3:9])[CH:3]=2)[CH:23]=[CH:22][CH:21]=1)=[O:17])[CH3:20]

参加物

7

反応物 5

HCID 1140TolueneHCID 72483,4-DimethylanilineHCID 11430Potassium CarbonateHCID 12388TridecaneHCID 10913723Ethyl 3-iododihydrocinnamate

生成物 1

HCID 18931917N,N-bis[3-(2-ethoxycarbonylethyl)phenyl]-3,4-xylidine

試薬・触媒・溶媒 1

HCID 24463Copper sulfate pentahydrate触媒

反応条件

温度
230 °C

実験手順

In a 100 ml-volume flask, 6 g of 3,4-xylidine, 34 g of ethyl 3-iododihydrocinnamate, 19 g of potassium carbonate, 5 g of copper sulfate pentahydrate and 20 ml of n-tridecane were placed, and the mixture was reacted under heating at 230° C. for 10 hours in a nitrogen stream. After the reaction, the system was cooled to room temperature, the reaction mixture was dissolved in 50 ml of toluene, insoluble matters were filtered, and the filtrate was purified by silica gel column chromatography using toluene to obtain 20 g of N, N-bis[3-(2-ethoxycarbonylethyl)phenyl]-3,4-xylidine as an oily substance. The IR spectrum of the product is shown in FIG. 1.

後処理

  1. customthe mixture was reacted
  2. customAfter the reaction
  3. temperaturethe system was cooled to room temperature
  4. filtrationinsoluble matters were filtered
  5. customthe filtrate was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-065831d99277499b89b8f6f92e86ad30
出典データセット
uspto-grants-1998_03
特許番号
US05731118

関連ノート

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