Hydrochloric Acid → HCID 69558143、化合物

HRID 1833166ノート

反応式

HRID 1833166 の反応式
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]

参加物

6

反応物 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

生成物 1

HCID 69558143HCID 69558143、化合物収率 32%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ad5b78ea5ea24115b18997e44db8506f
出典データセット
uspto-grants-2006_06
特許番号
US07067529B2

反応ノート

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