تفاعل #833523

ord-f9244171a8b7484b9ca410d55842088e

معادلة التفاعل

O
water
OCCCCCCCl
6-chlorohexanol
CC(=O)O
acetic acid
c1ccncc1
pyridine
CC(=O)OCCCCCCCl
6-acetoxy chlorohexane

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
10°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthey were refluxed for 2 hours
  2. 2
    workup.ADDITIONwas further added
  3. 3
    غسيلAfter neutralization the toluene layer with an aqueous saturated solution of sodium carbonate, it was washed with a small amount of water
  4. 4
    تجفيفfurther dried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONToluene and unreacted ingredients were distilled off from the toluene layer
  6. 6
    أخرىto obtain concentrates
  7. 7
    workup.DISTILLATIONThe concentrates were purified by distillation under a reduced pressure

الإجراء التجريبي

6-chlorohexanol (800 g) was added to anhydrous acetic acid (1,200 mL) cooled to 10° C. in an ice bath, and then pyridine (934 g) was dropped for 10 minutes. After the completion of dropping, they were refluxed for 2 hours. The reaction mixture was poured into water and toluene was further added and stirred. After neutralization the toluene layer with an aqueous saturated solution of sodium carbonate, it was washed with a small amount of water and further dried over anhydrous magnesium sulfate. Toluene and unreacted ingredients were distilled off from the toluene layer to obtain concentrates. The concentrates were purified by distillation under a reduced pressure to obtain 6-acetoxy chlorohexane (983 g). The boiling point was 82° C./5.3 hPa.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07393569B2uspto-grants-2008_07