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

HRID 49783

반응식

HRID 49783 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-791c61bd4d46488d9cd3f88bc69b7774
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710043B1

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