反応式
[CH:1]12[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH:2]1[OH:11])[CH2:8]2.[Cl:12][C:13](Cl)([O:15]C(=O)OC(Cl)(Cl)Cl)Cl.N1C=CC=CC=1>C(Cl)Cl>[Cl:12][C:13]([O:11][CH:2]1[CH:3]2[CH2:9][CH:7]3[CH2:6][CH:5]([CH2:10][CH:1]1[CH2:8]3)[CH2:4]2)=[O:15]参加物
5
実験手順
To a solution of 2-adamantanol (912 mg, 5.99 mmol) in methylene chloride (15 mL), at 0° C. under nitrogen, was added a solution of triphosgene (653 mg, 2.2 mmol) and pyridine (484 μL, 5.99 mmol) in methylene chloride. The reaction mixture was stirred at ambient temperature for 3 hours and then concentrated to dryness under reduced pressure. Ethyl acetate was added to the residue and the resultant mixture was filtered. The filtrate was concentrated in vacuo to give 980 mg of the title compound as a white powder. 1H NMR (CDCl3) δ1.5-2.2 (m, 14H), 5.02 (m, 1H).
後処理
- concentrationconcentrated to dryness under reduced pressure
- additionEthyl acetate was added to the residue
- filtrationthe resultant mixture was filtered
- concentrationThe filtrate was concentrated in vacuo
出典と根拠
- ORDレコード
- ord-7542839594044763989280a129f3bb2e
- 出典データセット
- uspto-grants-1993_12
- 特許番号
- US05270302
関連ノート
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