Hydrochloric Acid → HCID 69558143, 화합물

HRID 1833166노트

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HRID 1833166 반응식
C(OC(=O)[N:5]([CH2:29][CH:30](OC)OC)[CH:6]([C:16]1[CH:21]=[CH:20][C:19]([O:22][CH2:23][CH2:24][CH2:25][OH:26])=[C:18]([O:27][CH3:28])[CH:17]=1)[CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[CH:9]=1)C.Cl.[C:37]([O:40][CH2:41][CH3:42])(=[O:39])C.CCCCCC>CC(C)=O.O>[CH2:41]([O:40][C:37]([N:5]1[CH:29]=[CH:30][C:21]2[C:16](=[CH:17][C:18]([O:27][CH3:28])=[C:19]([O:22][CH2:23][CH2:24][CH2:25][OH:26])[CH:20]=2)[CH:6]1[CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[CH:9]=1)=[O:39])[CH3:42]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 21226206Ethyl acetate hexaneHCID 69552487(2,2-Dimethoxy-ethyl)-[1-[4-(3-hydroxy-propoxy)-3-methoxy-phenyl]-2-(3-methoxy-phenyl)-ethyl]-carbamic acid ethyl ester

생성물 1

HCID 69558143HCID 69558143, 화합물수율 32%

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

To a stirred solution of crude (2,2-dimethoxy-ethyl)-[1-[4-(3-hydroxy-propoxy)-3-methoxy-phenyl]-2-(3-methoxy-phenyl)-ethyl]-carbamic acid ethyl ester in acetone (30 mL) was added 6N hydrochloric acid (10 mL) at 0° C. The reaction mixture was stirred at room temperature for 15 hrs. The mixture was diluted with water. The solvent was evaporated and the aqueous layer was extracted with ethyl acetate (3×30 mL). The combined extracts were washed with saturated aqueous sodium chloride solution (20 mL), dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. Flash chromatography (Merck Silica gel 60, 70–230 mesh, 50% ethyl acetate/hexane) afforded 6-(3-hydroxy-propoxy)-7-methoxy-1-(3-methoxy-benzyl)-1H-isoquinoline-2-carboxylic acid ethyl ester (130, 32% yield in two steps) as a colorless oil.

후처리

  1. customThe solvent was evaporated
  2. extractionthe aqueous layer was extracted with ethyl acetate (3×30 mL)
  3. washThe combined extracts were washed with saturated aqueous sodium chloride solution (20 mL)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ad5b78ea5ea24115b18997e44db8506f
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07067529B2

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