4-Fluorophenyl isocyanate → N-(1-acetylpiperidin-4-yl)-N'-(4-fluorophenyl)urea

HRID 49783

反応式

HRID 49783 の反応式
Cl.[C:2]([N:5]1[CH2:10][CH2:9][CH:8]([NH2:11])[CH2:7][CH2:6]1)(=[O:4])[CH3:3].[F:12][C:13]1[CH:18]=[CH:17][C:16]([N:19]=[C:20]=[O:21])=[CH:15][CH:14]=1.C(N(C(C)C)CC)(C)C>ClCCl>[C:2]([N:5]1[CH2:10][CH2:9][CH:8]([NH:11][C:20]([NH:19][C:16]2[CH:17]=[CH:18][C:13]([F:12])=[CH:14][CH:15]=2)=[O:21])[CH2:7][CH2:6]1)(=[O:4])[CH3:3]

参加物

5

反応物 3

HCID 709554-Fluorophenyl isocyanateHCID 81531DiisopropylethylamineHCID 172216421-Acetyl-4-aminopiperidine hydrochloride

生成物 1

HCID 9860476N-(1-acetylpiperidin-4-yl)-N'-(4-fluorophenyl)urea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of 1-acetyl-4-aminopiperidine hydrochloride (536 mg) in dichloromethane (5 ml) were added 4-fluorophenyl isocyanate (375 μl) and diisopropylethylamine (575 μl ) at ambient temperature. After stirring for 3 hours, the reaction mixture was diluted with dichloromethane. An organic phase was separated and an aqueous phase was extracted with dichloromethane. A combined organic phase was dried over magnesium sulfate and the solvents were removed under reduced pressure. After crystallization from diisopropyl ether and n-hexane, N-(1-acetylpiperidin-4-yl)-N′-(4-fluorophenyl)urea (448 mg) was obtained.

後処理

  1. customAn organic phase was separated
  2. extractionan aqueous phase was extracted with dichloromethane
  3. dry with materialA combined organic phase was dried over magnesium sulfate
  4. customthe solvents were removed under reduced pressure
  5. customAfter crystallization from diisopropyl ether and n-hexane

出典と根拠

ORDレコード
ord-791c61bd4d46488d9cd3f88bc69b7774
出典データセット
uspto-grants-2004_03
特許番号
US06710043B1

関連ノート

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