Ethanol → Phenyl isocyanate

HRID 2351099ノート

反応式

HRID 2351099 の反応式
[C:1]1([NH:7][C:8](N(CC)CC)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.N1C=CC=CC=1.C(O)C>CC1C=CC=CC=1C>[C:1]1([N:7]=[C:8]=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 702EthanolHCID 1049PyridineHCID 13906N,N-Diethyl-N'-phenylurea

生成物 1

HCID 7672Phenyl isocyanate

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
114 °C

実験手順

A mixture of 1.95 g (10.1 mmoles) of 1-phenyl-3, 3-diethylurea and 3.24 g, (43.2 mmoles) of pyridine in 100 g of o-xylene was added to a 250 ml round bottom flask fitted with a magnetic stirrer, condenser, and a thermocouple for measuring reaction temperature. A nitrogen atmosphere was maintained over the reaction mixture. The mixture was heated to 114° C. for 60 minutes. A sample was taken from the flask and analyzed by infrared spectroscopy. There was no peak for the NCO band in the spectrum. Another sample was taken and reacted with ethanol. Any phenyl isocyanate that would have been formed would be converted to the carbamate derivative. This sample was then analyzed by high pressure liquid chromatography (HPCL). Only unreacted starting material was observed confirming that no thermal decomposition of the urea to isocyanate occurred.

後処理

  1. additionwas added to a 250 ml round bottom flask
  2. customfitted with a magnetic stirrer, condenser
  3. customreaction temperature
  4. temperatureA nitrogen atmosphere was maintained over the reaction mixture

出典と根拠

ORDレコード
ord-17f294fc613d4357a908fbe63ccd1e26
出典データセット
uspto-grants-1989_10
特許番号
US04871871

反応ノート

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