تفاعل #1256743

ord-b92f8a893a6b4bbb9a3f7e70a4b33521

معادلة التفاعل

[Cl-].[NH4+]
ammonium chloride
CCCCC
n-pentane
CC(C)[SiH](Cl)C(C)C
Diisopropylchlorosilane
C1CCOC1
THF
CC(C)C[SiH](C(C)C)C(C)C
Isobutyldiisopropylsilane

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITThe reaction mixture was left
  2. 2
    درجة الحرارةto cool
  3. 3
    غسيلThe formed organic layer was washed three times with water
  4. 4
    تجفيفby drying over sodium sulfate anhydrate
  5. 5
    أخرىThe solvent was removed
  6. 6
    workup.DISTILLATIONfollowed by purification through distillation under reduced pressure, whereby the Compound 40a
  7. 7
    أخرىwas obtained as a colorless liquid (boiling point; 70 mmHg, 102 to 106° C. fraction, 8.26 g, 50%)

الإجراء التجريبي

Diisopropylchlorosilane (16.4 mL, 96.1 mmol) was dissolved in THF (100 mL), and isobutylmagnesium bromide THF solution (1.0M, 100 mL) was added dropwise thereto under nitrogen for 30 minutes. Subsequently, cuprous bromide (286 mg, 2.00 mmol) was added to the resultant mixture, followed by stirring at 70° C. overnight. The reaction mixture was left to cool, and saturated aqueous ammonium chloride and n-pentane were added thereto. The formed organic layer was washed three times with water and once with saturated brine, followed by drying over sodium sulfate anhydrate. The solvent was removed, followed by purification through distillation under reduced pressure, whereby the Compound 40a was obtained as a colorless liquid (boiling point; 70 mmHg, 102 to 106° C. fraction, 8.26 g, 50%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07825103B2uspto-grants-2010_11