Potassium Iodide → 4-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester

HRID 511065노트

반응식

HRID 511065 반응식
[CH2:1]([O:3][C:4](=[O:9])[CH2:5][CH2:6][CH2:7]Br)[CH3:2].C(N(CC)CC)C.[F:17][C:18]([F:32])([F:31])[C:19]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[CH:21][CH:20]=1.[I-].[K+]>O1CCCC1.ClCCl>[CH2:1]([O:3][C:4](=[O:9])[CH2:5][CH2:6][CH2:7][N:28]1[CH2:27][CH2:26][N:25]([C:22]2[CH:21]=[CH:20][C:19]([C:18]([F:31])([F:32])[F:17])=[CH:24][CH:23]=2)[CH2:30][CH2:29]1)[CH3:2]

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 8471TriethylamineHCID 76300Ethyl 4-bromobutyrateHCID 1217181-(4-(Trifluoromethyl)phenyl)piperazine

생성물 1

HCID 585765934-[4-(4-Trifluoromethyl-phenyl)-piperazin-1-yl]-butyric acid ethyl ester수율 98%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl-4-bromobutyrate (390 mg, 2.00 mmol) and triethylamine (280 μL; 2.00 mmol) were added to a solution of 1-(4-trifluoromethylphenyl)-piperazine (460 mg; 2.00 mmol) in tetrahydrofuran (3 mL). Potassium iodide (332 mg; 2.00 mmol) was added and the resulting suspension is irradiated in a mono-mode microwave oven for 2 hours at 100° C. The suspension is then diluted with dichloromethane (15 mL) and washed twice with water (5 mL). The organic phase is then dried over sodium sulphate and is concentrated under reduced pressure to afford the desired product (660 mg; 1.96 mmol).

후처리

  1. customthe resulting suspension is irradiated in a mono-mode microwave oven for 2 hours at 100° C
  2. washwashed twice with water (5 mL)
  3. dry with materialThe organic phase is then dried over sodium sulphate
  4. concentrationis concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3760a034e1e54b5895f97400fcb86c3d
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096524B2

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