HRID851675
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 15 (52 mg, 0.025 mmol) in methanol-water-triethylamine 5:4:1 (v/v/v, 1 ml) is kept for 3 hours at room temperature, and evaporated in vacuo to a residue that is put on a Sephadex G-15 column and eluted with water. Fractions 1-4 (12 ml), eluted after blue dextran, are collected and lyophilized to give 16 (25.1 mg, 71%): [α]D27 +96.2° (c 1.0, H2O); NMR (D2O)δ: 5.37 (s, 1H, H-1), 5.34 (s, 3H, H-1) 4.34 (2H), 4.18 (1H) (α-CH), 3.22 (m, ε-CH2), 2.93 (m, SCH2), 2.70 (t, 2H), 2.60 (t, 6H) (SCH2CH2), 1.34-1.94 (CCH2CH2CH2C).
WORKUP
后处理
- customevaporated in vacuo to a residue that
- washeluted with water
- washFractions 1-4 (12 ml), eluted after blue dextran
- customare collected