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Potassium Carbonate → HCID 22503186, 화합물

HRID 1814592
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HRID 1814592 반응식
[CH2:1]([O:8][CH2:9][CH2:10][O:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[NH:19][C:20](=O)[C:21]3[C:26]([CH:27]=2)=[CH:25][CH:24]=[CH:23][CH:22]=3)=[C:14]([O:29][CH3:30])[CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:31]([N:33]1[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]1)[CH3:32].C(=O)([O-])[O-].[K+].[K+].P(Cl)(Cl)([Cl:47])=O>>[ClH:47].[CH2:31]([N:33]1[CH2:38][CH2:37][N:36]([C:20]2[C:21]3[C:26](=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH:27]=[C:18]([C:15]3[CH:16]=[CH:17][C:12]([O:11][CH2:10][CH2:9][O:8][CH2:1][C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=4)=[CH:13][C:14]=3[O:29][CH3:30])[N:19]=2)[CH2:35][CH2:34]1)[CH3:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 11430Potassium CarbonateHCID 24813Phosphorus oxychlorideHCID 791961-EthylpiperazineHCID 22503579HCID 22503579, 화합물

생성물 1

HCID 22503186HCID 22503186, 화합물

실험 절차

The resulting 3-[4-(2-benzyloxyethoxy)-2-methoxyphenyl]isoquinolin-1-one (0.47 g) was added to phosphorus oxychloride (10 ml), and the mixture was reacted at room temperature overnight. The reaction solution was evaporated, and to the resulting residue were added ethyl acetate and purified water. The ethyl acetate layer was washed with water, an aqueous solution of sodium bicarbonate and brine, and dried over magnesium sulfate. The solvent was evaporated, and the resulting 1-chloro-3-[4-(2-benzyloxyethoxy)-2-methoxyphenyl]isoquinoline was reacted as it was with N-ethylpiperazine (5 ml) in the presence of potassium carbonate (1.2 g) at 120° C. for 24 hr. The reaction solution was evaporated, and to the resulting residue were added ethyl acetate and purified water. The ethyl acetate layer was washed with water and brine, and dried over magnesium sulfate. The solvent was evaporated, and the resulting residue was purified by NH-silica gel column chromatography (ethyl acetate/hexane system), to give 1-(4-ethylpiperazin-1-yl)-3-[4-(2-benzyloxyethoxy)-2-methoxyphenyl]isoquinoline hydrochloride (0.11 g) as a yellow powder.

후처리

  1. customthe mixture was reacted at room temperature overnight
  2. customThe reaction solution was evaporated
  3. additionto the resulting residue were added ethyl acetate
  4. custompurified water
  5. washThe ethyl acetate layer was washed with water
  6. dry with materialan aqueous solution of sodium bicarbonate and brine, and dried over magnesium sulfate
  7. customThe solvent was evaporated
  8. customthe resulting 1-chloro-3-[4-(2-benzyloxyethoxy)-2-methoxyphenyl]isoquinoline was reacted as it
  9. customThe reaction solution was evaporated
  10. additionto the resulting residue were added ethyl acetate
  11. custompurified water
  12. washThe ethyl acetate layer was washed with water and brine
  13. dry with materialdried over magnesium sulfate
  14. customThe solvent was evaporated
  15. customthe resulting residue was purified by NH-silica gel column chromatography (ethyl acetate/hexane system)

출처 및 근거

ORD 기록
ord-025cf10e51304a2994a19a658bd99d48
출처 데이터셋
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06875761B2

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