HRID225841

反应详情

EQUATION

反应方程式

HRID 225841 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of methyl (1-methyl-1H-indazolecarboxylate (3.88 g, 20.4 mmole) in 40% aqueous CH3NH2 (100 mL) and MeOH (5 mL) was stirred at RT for 4 hr. During that time the suspension became a solution. The mixture was concentrated to approximately ⅓ by volume at which time the product precipitated as a pale yellow solid. The solid was collected by filtration, washed with H2O, and dried in vacuo to give the title compound (3.42 g, 89%) which was sufficiently pure for use in the next step: 1H NMR (300 MHz, CDCl3) δ 8.24 (m, 1 H), 7.47 (m, 2 H), 7.34 (m, 1 H), 6.95 (bs, 1 H), 4.19 (s, 3 H), 3.05 (d, J=12.0 Hz, 3 H).

WORKUP

后处理

  1. concentrationThe mixture was concentrated to approximately ⅓ by volume at which time the product
  2. customprecipitated as a pale yellow solid
  3. filtrationThe solid was collected by filtration
  4. washwashed with H2O
  5. customdried in vacuo