HRID2090342

反应详情

EQUATION

反应方程式

HRID 2090342 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Iodotrimethylsilane (0.982 mL, 0.00690 mol, Aldrich, Cat. No. 195529) was added to a solution of methyl 7-bromo-3-methyl-3,4-dihydroisoquinoline-2(1H)-carboxylate (490 mg, 0.0017 mol) in methylene chloride (10 mL) and the reaction was stirred at 50° C. for 2 h. The reaction was cooled to r.t. and anhydrous methanol (2 mL) was added. The reaction mixture was stirred for additional 5 min, and the volatiles were removed under reduced pressure. The residue was treated with diethyl ether and filtered. The solid was washed with ether, dried under vacuum to provide the desired compound which was directly used in the next step reaction without further purification. LCMS (M+H)+: m/z=226.2.

WORKUP

后处理

  1. temperatureThe reaction was cooled to r.t.
  2. stirringThe reaction mixture was stirred for additional 5 min
  3. customthe volatiles were removed under reduced pressure
  4. additionThe residue was treated with diethyl ether
  5. filtrationfiltered
  6. washThe solid was washed with ether
  7. customdried under vacuum