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Potassium Carbonate → HCID 16123291, 화합물

HRID 2063309
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HRID 2063309 반응식
[C:1]1([CH:7]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:8]2[CH2:11][CH:10]([N:12]3[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]3)[CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])([O-])=O.[K+].[K+].[C:30](Cl)(=[O:33])[CH2:31][CH3:32]>C(#N)C>[C:18]1([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[N:8]2[CH2:9][CH:10]([N:12]3[CH2:17][CH2:16][N:15]([C:30](=[O:33])[CH2:31][CH3:32])[CH2:14][CH2:13]3)[CH2:11]2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 62324Propionyl chlorideHCID 161232921-[1-(Diphenylmethyl)azetidin-3-yl]piperazine

생성물 1

HCID 16123291HCID 16123291, 화합물수율 73.4%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 1-[1-(diphenylmethyl)azetidin-3-yl]piperazine (250 mg, 0.81 mmol), K2CO3 (146 mg, 1.1 mmol), propionyl chloride (98 mg, 1.1 mmol) and acetonitrile (6 mL) was stirred at RT for 16 h. The mixture was filtered through a phase separator column and the solvent was removed by evaporation. The residue was dissolved in methylene chloride and the solution washed with aqueous NaHCO3. The organic phase was separated by using a phase separator column and then the solvent was removed by evaporation. There was obtained 216 mg (73%) of 1-[1-(diphenylmethyl)azetidin-3-yl]-4-propionylpiperazine as an oil. 1H NMR (500 MHz, CDCl3): 1.1-1.2 (t, 3H), 2.2-2.4 (m, 6H), 2.9 (t, 2H), 3.0 (m, 1H), 3.4-3.5 (m, 4H), 3.6 (b, 2H), 4.4 (s, 1H), 7.2 (m, 2H), 7.3 (m, 4H), 7.4 (m, 4H); LCMS: m/z 364 (M+1)+.

후처리

  1. filtrationThe mixture was filtered through a phase separator column
  2. customthe solvent was removed by evaporation
  3. dissolutionThe residue was dissolved in methylene chloride
  4. washthe solution washed with aqueous NaHCO3
  5. customThe organic phase was separated
  6. customthe solvent was removed by evaporation

출처 및 근거

ORD 기록
ord-700a77b4f085497ebaf1a0559600f645
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288370B2

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