反応式
C[C:2]1(C)[CH2:11][CH2:10][CH:9](O)[C:8]2[CH:7]=[C:6]([C:13]3[CH:14]=[C:15]4[C:20](=[CH:21][CH:22]=3)[CH:19]=[C:18]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:17]=[CH:16]4)[CH:5]=C[C:3]1=2.CCN([CH:35]([CH3:37])[CH3:36])C(C)C.[CH3:38][O:39][CH2:40]Cl.[I-].C([NH3+])(C)(C)C.[OH2:48]>C(Cl)Cl.C(OCC)(=O)C>[CH2:26]([O:25][C:23]([C:18]1[CH:17]=[CH:16][C:15]2[C:20](=[CH:21][CH:22]=[C:13]([CH:6]3[CH:7]([O:48][CH2:40][O:39][CH3:38])[C:8]4[CH:3]=[CH:2][CH:11]=[CH:10][C:9]=4[C:35]([CH3:36])([CH3:37])[CH2:5]3)[CH:14]=2)[CH:19]=1)=[O:24])[CH3:27]参加物
8
反応物 5
生成物 1
試薬・触媒・溶媒 2
実験手順
To a cold (0° C.) solution of 130 mg (0.35 mmol) of ethyl-6-[5,6,7,8-tetrahydro-5,5-dimethyl-8-(hydroxy)-naphth-7-yl]naphth-2-oate (Compound B4) in 2.0 mL of methylene chloride was added 50 mg (0.15 mL, 0.86 mmol) of Hunig's base, followed by 0.21 g (0.20 mL, 2.6 mmol) chloromethyl methyl ether was added and stirred at room temperature for 14 h. About 500 mgs of t-butylammonium iodide was then added and the reaction was warmed to 35° C. for one additional hour. The reaction was diluted with water, and extracted with CH2Cl2 (2×). The combined organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo to give an oil. The title compound was obtained as an oil after flash chromatography (silica, 10% ethyl acetate).
後処理
- additionwas added
- temperaturethe reaction was warmed to 35° C. for one additional hour
- extractionextracted with CH2Cl2 (2×)
- washThe combined organic layer was washed with brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
- customto give an oil
出典と根拠
- ORDレコード
- ord-817b42e28a814120a186adbd9a83052d
- 出典データセット
- uspto-grants-1999_12
- 特許番号
- US05998655
関連ノート
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