Ethanol → Phenyl isocyanate

HRID 2351099노트

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HRID 2351099 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 7672Phenyl isocyanate

시약·촉매·용매 1

HCID 7237O-Xylene용매

반응 조건

온도
114 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-17f294fc613d4357a908fbe63ccd1e26
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04871871

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