HRID29472

反应详情

EQUATION

反应方程式

HRID 29472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of methyl N-[(4′-{[4-(3-methoxypropyl)-3-methyl-1-benzofuran-2-yl]methoxy}-1,1′-biphenyl-4-yl)sulfonyl]-L-valinate (192 mg, 0.331 mmol) in tetrahydrofuran (12 mL), methanol (8 mL), water (4 mL) was added lithium hydroxide (317 mg, 13.25 mmol). After stirring for 2.5 days at room temperature hydrochloric acid (13.25 mL, 1 N solution) was added followed by ethyl acetate (80 mL). The layers were separated and the organic phase was washed with water, dried over sodium sulfate, filtered and reduced to dryness. The solid material was recrystallized from a minimum amount of boiling isopropanol to furnish which furnished 171 mg (91%) of N-[(4′-{[4-(3-methoxypropyl)-3-methyl-1-benzofuran-2-yl]methoxy}-1,1′-biphenyl-4-yl)sulfonyl]-L-valine as a white solid. MS (ES) m/z: 564.2 (M−H), 1129.4 (2M−H).

WORKUP

后处理

  1. additionwas added
  2. customThe layers were separated
  3. washthe organic phase was washed with water
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. customThe solid material was recrystallized from a minimum amount of boiling isopropanol
  7. customto furnish which