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Sodium Carbonate → HCID 19911439, 화합물

HRID 1533926
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HRID 1533926 반응식
[CH2:1]([C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1)[CH3:2].[Cl:15][CH2:16][CH2:17][CH:18]1[O:22][C:21](=[O:23])[N:20]([CH3:24])[CH2:19]1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)CCC.[I-].[K+]>[ClH:15].[ClH:15].[CH2:1]([C:3]1[CH:4]=[C:5]([N:9]2[CH2:10][CH2:11][N:12]([CH2:16][CH2:17][CH:18]3[O:22][C:21](=[O:23])[N:20]([CH3:24])[CH2:19]3)[CH2:13][CH2:14]2)[CH:6]=[CH:7][CH:8]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 146987465-(2-Chloro-ethyl)-3-methyl-oxazolidin-2-oneHCID 199114731-(3-Ethylphenyl)piperazine

생성물 1

HCID 19911439HCID 19911439, 화합물수율 139.7%

시약·촉매·용매 2

HCID 4875Potassium Iodide촉매HCID 2631-Butanol
용매

실험 절차

A mixture of 12.2 g (0.064 mol) of 1-(3-ethylphenyl)piperazine, 12.6 g (0.077 mol) of 5-(2-chloroethyl)-3-methyl-2-oxazolidinone, 27.1 g (0.255 mol) of anhydrous sodium carbonate, and 0.5 g (0.003 mol) of potassium iodide in 300 mL of 1-butanol was heated at reflux for 16 h. The mixture was concentrated under reduced pressure and the residue partitioned between 300 mL of benzene and 300 mL of water. The benzene layer was washed with water and brine, dried (MgSO4) and concentrated under reduced pressure to yield 21.0 g (100%) of a gold-colored, viscous oil.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 16 h
  3. concentrationThe mixture was concentrated under reduced pressure
  4. customthe residue partitioned between 300 mL of benzene and 300 mL of water
  5. washThe benzene layer was washed with water and brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-eb28ad34538d45dfb58fdff58c3978d1
출처 데이터셋
uspto-grants-1992_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05086055

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