反応 #75234

ord-abea3c8d56614949a76c3cd6cd77318a

反応方程式

CC(C)=CCC/C(C)=C/CC/C(C)=C/CC/C(C)=C/CC/C(C)=C/CC/C(C)=C/CC/C(C)=C/CC/C(C)=C/CC/C(C)=C/CO
solanesol
O=C([O-])O.[Na+]
sodium hydrogencarbonate
CCCCCCCCCCCCCCCCCC(=O)O
stearic acid
CCCCCCCCCCCCCCCCCC(=O)OCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)CCC=C(C)C
3,7,11,15,19,23,27,31,35-Nonamethyl-2,6,10,14,18,22,26,30,34-hexatriacontanonaenyl stearate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the solution was refluxed
  2. 2
    その他After completion of the reaction
  3. 3
    workup.ADDITIONadded with about 10 g
  4. 4
    抽出After extraction with ether
  5. 5
    洗浄the ether layer was washed with water
  6. 6
    workup.DISTILLATIONsubjected to distillation under reduced pressure
  7. 7
    その他The residual oily substance was purified by column chromatography with 100 g
  8. 8
    その他of silica gel to obtain 12.5 g

実験手順

16 Grams of solanesol, 7.5 g. of stearic acid and 10 g. of polyphosphoric acid ethyl ester were dissolved in 40 ml of chloroform and the solution was refluxed under stirring for 4 hours. After completion of the reaction, the reaction product was poured in water and added with about 10 g. of sodium hydrogencarbonate to decompose the polyphosphoric acid ester. After extraction with ether, the ether layer was washed with water and subjected to distillation under reduced pressure. The residual oily substance was purified by column chromatography with 100 g. of silica gel to obtain 12.5 g. (54.8%) of white solid (m.p. 36°-37° C.).______________________________________Elementary analysis as C63H108O2 : C H______________________________________Theoretical (%): 84.31 12.13Found (%): 84.27 12.11______________________________________

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04175139uspto-grants-1979_11