Potassium Carbonate → HCID 11529282, 화합물

HRID 1483890노트

반응식

HRID 1483890 반응식
[CH3:1][S:2]([C:5]1[CH:6]=[C:7]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)[CH:8]=[CH:9][CH:10]=1)(=[O:4])=[O:3].C([O-])([O-])=O.[K+].[K+].I[CH2:24][CH2:25][CH3:26]>CC#N>[CH3:1][S:2]([C:5]1[CH:6]=[C:7]([N:11]2[CH2:16][CH2:15][N:14]([CH2:24][CH2:25][CH3:26])[CH2:13][CH2:12]2)[CH:8]=[CH:9][CH:10]=1)(=[O:3])=[O:4]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 336431-IodopropaneHCID 129889541-(3-(Methylsulfonyl)phenyl)piperazine

생성물 1

HCID 11529282HCID 11529282, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A suspension of 1-(3-methanesulfonyl-phenyl)-piperazine (350 mg) and ground K2CO3 (403 mg) was stirred in CH3CN (25 mL) at room temperature. 1-Iodopropane (712 μL) was added. The mixture was refluxed overnight. The reaction mixture was filtered and the volatiles were evaporated in vacuum. The oily residue was chromatographed on a silica column with MeOH:CH2Cl2 (1:30 (v/v)) as eluent. Collection of the fractions containing pure product and evaporation of the solvent afforded pure 1-(3-methanesulfonyl-phenyl)-4-propyl-piperazine (220 mg). The amine was converted into the HCl salt and recrystallized from ethanol/diethylether: m.p. 233° C. MS m/z (relative intensity, 70 eV) 282 (M+, 30), 254 (15), 253 (bp), 210 (17), 70 (21).

후처리

  1. temperatureThe mixture was refluxed overnight
  2. filtrationThe reaction mixture was filtered
  3. customthe volatiles were evaporated in vacuum
  4. customThe oily residue was chromatographed on a silica column with MeOH:CH2Cl2 (1:30 (v/v)) as eluent
  5. customCollection of the fractions
  6. additioncontaining pure
  7. customproduct and evaporation of the solvent

출처 및 근거

ORD 기록
ord-ad6130eaa88544b29a1fd56f8d7ed83e
출처 데이터셋
uspto-grants-2016_08
특허 번호
USRE046117E1

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