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 ethyl 3,4-bis(benzyloxy)-5-(dimethylcarbamoyl)-1-(4-hydroxyphenyl)-1H-pyrrole-2-carboxylate (36) (30 mg, 0.06 mmol) in MeOH (2 mL) was passed through a Thales ‘H-cube’ cartridge (10% Pd/C) at a flow rate of 1 mL/min at 25° C. under H2 (full H2 mode). The output was concentrated in vacuo, and a solid was collected by filtration after trituration with isohexane to afford ethyl 5-(dimethylcarbamoyl)-3,4-dihydroxy-1-(4-hydroxyphenyl)-1H-pyrrole-2-carboxylate (UL1-100) (11 mg, 56%) as a yellow solid: m/z 335 (M+H)+ (ES+), 333 (M−H)− (ES−). 1H NMR (400 MHz, DMSO-d6) δ: 9.50 (s, 1H), 8.54 (s, 1H), 8.42 (s, 1H), 6.94-6.86 (m, 2H), 6.69-6.62 (m, 2H), 3.99 (q, J=7.0 Hz, 2H), 2.81 (br s, 6H), 0.98 (t J=7.0 Hz, 3H).
WORKUP
后处理
- customat 25° C.
- concentrationThe output was concentrated in vacuo
- filtrationa solid was collected by filtration after trituration with isohexane