反応 #4016

ord-3f1521d404b14cd4bf43a059b7950a8c

反応方程式

CCOC(C)(OCC)OCC
1,1,1-triethoxyethane
O=C1CCC(=O)N1Cl
N-chlorosuccinimide
CCOC(CCl)(OCC)OCC
2-chloro-1,1,1-triethoxyethane
収率 77.1%

反応条件

温度
40°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他irradiated with an ultraviolet lamp
  2. 2
    その他subsided upon completion of the reaction
  3. 3
    ろ過The precipitated succinimide byproduct was filtered off
  4. 4
    濃縮the filtrate was concentrated
  5. 5
    その他to remove carbon tetrachloride
  6. 6
    workup.DISTILLATIONThe residual liquid was distilled

実験手順

A mixture of 1,1,1-triethoxyethane (97.3 g) and N-chlorosuccinimide (88.1 g) in carbon tetrachloride (600 ml) was warmed to 40° C. and then irradiated with an ultraviolet lamp. The reaction became exothermic and then subsided upon completion of the reaction. The precipitated succinimide byproduct was filtered off and the filtrate was concentrated to remove carbon tetrachloride. The residual liquid was distilled to obtain pure 2-chloro-1,1,1-triethoxyethane (91.0 g; b.p. 91° C./25 mm).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04723010uspto-grants-1988_02