反応式
Cl[CH2:2][C@H:3]1[O:8][C:7]([CH3:10])([CH3:9])[O:6][C@@H:5]([CH2:11][C:12]([OH:14])=[O:13])[CH2:4]1.[CH3:15][C:16](Cl)([CH3:18])[CH3:17]>C([O-])(=O)C.C([N+](CCCC)(CCCC)CCCC)CCC.CN1CCCC1=O>[C:7]([O:8][CH2:2][C@H:3]1[O:8][C:7]([CH3:10])([CH3:9])[O:6][C@@H:5]([CH2:11][C:12]([O:14][C:16]([CH3:18])([CH3:17])[CH3:15])=[O:13])[CH2:4]1)(=[O:6])[CH3:9]参加物
反応物 1
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 85 °C
実験手順
Solid tetra-n-butylammonium acetate prepared in step (e)(i) of Example 1 above (106.2 g, 0.352 mole) was added in one portion to a mechanically stirred solution of the chloride (4R-cis)-6-(chloromethyl)-2,2-dimethyl-1,3-dioxane-4-acetic acid, 1,1-dimethylethyl ester prepared in step (d) of Example 1 above (32.7 g, 0.117 mole) in HPLC grade 1-methyl-2-pyrrolidinone (471 ml) under argon. The resulting solution was stirred at 85° C. (internal temperature). After 30 to 60 minutes the reaction mixture became homogeneous and brown in color. The progress of the reaction was followed by TLC and GC analysis. (TLC: Rf =0.54 for the title compound; Rf =0.63 for the chloride starting material (silica gel, Ethyl acetate:Hexane, 1:1, visualization by Ce(SO4)2 spray).) After 9 hours the reaction was completed.
出典と根拠
- ORDレコード
- ord-dcc8fdcf516f4de2951ab062d0b48ccd
- 出典データセット
- uspto-grants-1994_01
- 特許番号
- US05278313
関連ノート
読み込み中…