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Hydrochloric Acid → HCID 19814218, 화합물

HRID 466595
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HRID 466595 반응식
Cl.[CH2:2]([N:9]1[CH2:14][CH2:13][C:12]([O:17][C:18](=[O:24])NCCCC)([C:15]#[CH:16])[CH2:11][CH2:10]1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[O:25]1CCOCC1>>[CH2:2]([N:9]1[CH2:10][CH2:11][C:12]2([O:17][C:18](=[O:24])[O:25][C:15]2=[CH2:16])[CH2:13][CH2:14]1)[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 19814307HCID 19814307, 화합물

생성물 1

HCID 19814218HCID 19814218, 화합물수율 80.6%

실험 절차

Dry gaseous hydrogen chloride is introduced at 20° to 50° C. during 2.5 to 3 hours into a solution containing 31.4 g of 1-benzyl-4-butylcarbamoyloxy-4-ethynylpiperidine in 157 ml of anhydrous dioxane. After standing overnight the reaction mixture is evaporated in a water bath of 40° to 50° C. temperature under reduced pressure. After adding 200 ml of water to the evaporation residue the base is liberated by sodium hydrogen carbonate. After filtration the solid precipitate is washed to chloride-free with water and dried. The crude product obtained is recrystallized from n-hexane under clarifying by activated carbon to give the title compound in 80.6% yield, m.p.: 65°-67° C.

후처리

  1. customthe reaction mixture is evaporated in a water bath of 40° to 50° C. temperature under reduced pressure
  2. additionAfter adding 200 ml of water to the evaporation residue the base
  3. filtrationAfter filtration the solid precipitate
  4. washis washed to chloride-free with water
  5. customdried
  6. customThe crude product obtained
  7. customis recrystallized from n-hexane under clarifying by activated carbon

출처 및 근거

ORD 기록
ord-f96868f33eb04fbf9eed659dcf49057a
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05157038

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