Phosgene → 2-Ethylhexyloxycarbonyl isocyanate

HRID 867979노트

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HRID 867979 반응식
[C:1](=[O:12])([O:3][CH2:4][CH:5]([CH2:10][CH3:11])[CH2:6][CH2:7][CH2:8][CH3:9])[NH2:2].[C:13](Cl)(Cl)=[O:14]>CCCCCCCCCCCCCCCCCCCNC=O.ClC1C=CC=CC=1>[CH2:10]([CH:5]([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:4][O:3][C:1]([N:2]=[C:13]=[O:14])=[O:12])[CH3:11]

참가 물질

5

반응물 2

HCID 6371Phosgene3회HCID 94289Carbamic acid, 2-ethylhexyl ester

생성물 1

HCID 139080002-Ethylhexyloxycarbonyl isocyanate수율 85%

시약·촉매·용매 2

HCID 17845310Methylstearylformamide촉매HCID 7964Chlorobenzene용매

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온도
-78 °C

실험 절차

138.6 g of 2-ethylhexyl carbamate were initially introduced in melted form and 93 g of phosgene were passed into the melt at 80° C. within 3.25 hours, the gas outlet stream being passed through a reflux condenser cooled to -78° C. 800 g of chlorobenzene and 5.0 g of methylstearylformamide were then added, the mixture was heaLed to 120° C., and 48 g of phosgene were passed into the mixture within 3 hours. The mixture was stirred for a further 1 hour at 130° C. and excess phosgene was subsequently blown out using nitrogen. Subsequent distillation produced 135.5 g (=85% of theory) of 2-ethylhexyloxycarbonyl isocyanate having a boiling point of 45°-60° C. at 0.13-0.4 mbar.

후처리

  1. customthe gas outlet stream being passed through a reflux condenser
  2. customwas heaLed to 120° C.
  3. distillationSubsequent distillation

출처 및 근거

ORD 기록
ord-a698b358b4e5427e8ede694b582186b2
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04777283

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