HRID2191005
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
Compound 6.4 (170 mg, 0.31 mmol) was dissolved in 90% TFA in H2O (10 mL). The mixture was stirred for 30 min and concentrated down under reduced pressure. The residue was subjected to a silica gel column chromatography eluting with 10% MeOH in CH2Cl2 to yield compound 6.5 (110 mg, 70% yield). 1HNMR (300 MHz, CD3OD) δ 1.24-1.28 (m, 6H), 3.96-4.06 (m, 4H), 4.63 (t, 1H, J=5.1), 4.73 (s, 1H), 4.97 (t, 1H, J=4.2), 5.92-6.04 (m, 1H), 6.5 (d, 1H, J=3.9), 6.81-6.96 (m, 1H), 7.55-8.12 (m, 5H), 8.77 (s, 1H). LRMS (ESI) MH+ C21H25N6O7P requires 505.2. Found 504.9.
WORKUP
后处理
- concentrationconcentrated down under reduced pressure
- washeluting with 10% MeOH in CH2Cl2