Phosgene → 2-Ethylhexyloxycarbonyl isocyanate

HRID 867979

反応式

HRID 867979 の反応式
[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]

参加物

5

反応物 2

HCID 6371Phosgene3 回HCID 94289Carbamic acid, 2-ethylhexyl ester

生成物 1

HCID 139080002-Ethylhexyloxycarbonyl isocyanate収率 85%

試薬・触媒・溶媒 2

HCID 17845310Methylstearylformamide触媒HCID 7964Chlorobenzene溶媒

反応条件

温度
-78 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-a698b358b4e5427e8ede694b582186b2
出典データセット
uspto-grants-1988_10
特許番号
US04777283

関連ノート

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