HRID1906114

反应详情

EQUATION

反应方程式

HRID 1906114 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 6-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)furo[2,3-b]pyridine-5-carboxylic acid (1.7 g 0.056 mol) and 1.0 g (0.0072 mol) potassium carbonate in 200 mL 9:1 ethanol:water is added to 100 mg 5% palladium on carbon catalyst in a 500 mL pressure bottle. The bottle is fitted to a Parr hydrogenation apparatus, pressurized to 30 psi, with hydrogen, then shaken at room temperature for 10 hours. The catalyst is removed by filtration through a sintered glass funnel, and the filtrate concentrated in vacuo to 10 mL. Acidification of the residue to pH 2 gives a white precipitate which is removed by filtration, washed with water and air dried to give 1.0 g (63%) of 2,3-dihydro-6-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)furo-[2,3-b]pyridine-5-carboxylic acid as an off-white solid, mp 189°-192° C.

WORKUP

后处理

  1. customThe bottle is fitted to a Parr hydrogenation apparatus
  2. customThe catalyst is removed by filtration through a sintered glass funnel
  3. concentrationthe filtrate concentrated in vacuo to 10 mL
  4. customAcidification of the residue to pH 2 gives a white precipitate which
  5. customis removed by filtration
  6. washwashed with water and air
  7. customdried