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Hydrochloric Acid → HCID 19814218、化合物

HRID 466595
ノート
印刷プレビュー

反応式

HRID 466595 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 19814307HCID 19814307、化合物

生成物 1

HCID 19814218HCID 19814218、化合物収率 80.6%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f96868f33eb04fbf9eed659dcf49057a
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05157038

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート