تفاعل #94089

ord-21400c26edc047e9a8a0994dfa4c8ee8

معادلة التفاعل

C1CCOC1
tetrahydrofuran
C1CCOC1
tetrahydrofuran
[Li][CH2]CCC
n-butyllithium
CCCCBr
n-butyl bromide
C1CSCSC1
1,3-dithiane
CCCCC1SCCCS1
title compound
CCCCC1SCCCS1
2-n-Butyl-1,3-dithiane

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىat -20° to -25° C
  2. 2
    workup.STIRRINGwas stirred for 1 hour at -20° to -25° C. and for a further 30 minutes at room temperture
  3. 3
    تركيزconcentrated under reduced pressure
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in diethyl ether
  5. 5
    غسيلwashed with water
  6. 6
    تجفيفan aqueous solution of sodium chloride, dried over magnesium sulphate
  7. 7
    تركيزconcentrated under reduced pressure
  8. 8
    أخرىto give 6.8 g

الإجراء التجريبي

30 ml. of a 1.6M solution of n-butyllithium in n-hexane were added dropwise to a solution of 4.8 g. of 1,3-dithiane in 150 ml. of tetrahydrofuran under an atmosphere of nitrogen at -20° to -25° C. After 2 hours stirring, 6 g. of n-butyl bromide in 60 ml. of tetrahydrofuran were added dropwise to the reaction mixture, which was stirred for 1 hour at -20° to -25° C. and for a further 30 minutes at room temperture and then concentrated under reduced pressure. The residue was dissolved in diethyl ether, washed with water and an aqueous solution of sodium chloride, dried over magnesium sulphate and concentrated under reduced pressure to give 6.8 g. of the title compound having the following physical characteristics:

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04128720uspto-grants-1978_12