Acetic Acid → 1-Hexanol, 6-chloro-, 1-acetate

HRID 602221노트

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HRID 602221 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][OH:8].[C:9](O)(=[O:11])[CH3:10].N1C=CC=CC=1.O>C1(C)C=CC=CC=1>[C:9]([O:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][Cl:1])(=[O:11])[CH3:10]

참가 물질

6

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온도
10 °C

실험 절차

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.

후처리

  1. temperaturethey were refluxed for 2 hours
  2. additionwas further added
  3. washAfter neutralization the toluene layer with an aqueous saturated solution of sodium carbonate, it was washed with a small amount of water
  4. dry with materialfurther dried over anhydrous magnesium sulfate
  5. distillationToluene and unreacted ingredients were distilled off from the toluene layer
  6. customto obtain concentrates
  7. distillationThe concentrates were purified by distillation under a reduced pressure

출처 및 근거

ORD 기록
ord-b8374db747bd4a80b17fb2f2af04a106
출처 데이터셋
uspto-grants-2011_03
특허 번호
USRE042221E1

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