Potassium Iodide → 1-[3,3-Bis(4-fluorophenyl)propyl]piperazine

HRID 2073482노트

반응식

HRID 2073482 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH2:9][CH2:10]Br)=[CH:4][CH:3]=1.[N:19]1(C(OCC)=O)[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[OH-].[K+]>C1(C)C=CC=CC=1.C(O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH2:9][CH2:10][N:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)=[CH:4][CH:3]=1

참가 물질

8

반응물 5

HCID 4875Potassium IodideHCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 11430Potassium CarbonateHCID 14797Potassium HydroxideHCID 138832773-Bromo-1,1-bis(4-fluorophenyl)propane

생성물 1

HCID 138832821-[3,3-Bis(4-fluorophenyl)propyl]piperazine수율 84.7%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 1140Toluene용매

실험 절차

31.1 g (0.100 mol) of 3,3-bis(4-fluorophenyl)propyl bromide, 20.6 g (0.130 mol) of ethyl piperazine-1-carboxylate, 27.6 g (0.200 mol) of powdered potassium carbonate and 4.15 g of potassium iodide were heated at the reflux temperature in 400 ml of toluene for 31 hours; the precipitate was then filtered off and the filtrate was concentrated. The material thus obtained was dissolved in 450 ml of ethanol, 450 ml of 4N KOH were added and the mixture was heated under reflux for 9 hours. After customary working up (compare Example 3d), 26.8 g of product, melting point 58°-64° C., were obtained.

후처리

  1. filtrationthe precipitate was then filtered off
  2. concentrationthe filtrate was concentrated
  3. customThe material thus obtained
  4. temperaturethe mixture was heated
  5. temperatureunder reflux for 9 hours

출처 및 근거

ORD 기록
ord-ca1feb9d1186454ab36772d0d5a42c07
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04918073

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