huagongshe.com
HRID1366741

反应详情

EQUATION

反应方程式

HRID 1366741 的结构方程式

REACTANTS

反应物

3
结构：CCN(CC)P1(=NC(C)(C)C)NCCCN1C
HCID19990018

未命名化合物

结构：Nc1nccc2cc(O)ccc12
HCID135753991

未命名化合物

结构：CC(C)(C)OC(=O)N[C@H]1CC[C@H](OS(C)(=O)=O)CC1
HCID178418975

未命名化合物

PRODUCTS

生成物

1
结构：CC(C)(C)OC(=O)N[C@H]1CC[C@@H](Oc2ccc3c(N)nccc3c2)CC1
HCID178454061

未命名化合物

收率 7.8%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC#N
溶剂HCID6342

Acetonitrile

C2H3N

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A suspension of 1-amino-6-hydroxyisoquinoline (0.08 g, 0.5mmol), methane-sulfonic acid trans-4-tert-butoxycarbonylaminocyclohexyl ester (176 mg) and 2-tert-butylimino-2-diethylamino-1,3-dimethyl-perhydro-1,3,2-diazaphosphorine on polystyrene (270mg, ˜2.2 mmol/g loading) in acetonitrile (2ml) were heated at 120° C. over a period of 15 minutes using the microwave. The excess supported reagent was removed by filtration, washing with acetonitrile followed by methanol, and the filtrate evaporated to dryness under reduced pressure. Purification was achieved by prep-HPLC to give cis-[4-(1-aminoisoquinolin-6-yloxy)cyclohexyl]carbamic acid tert-butyl ester (14 mg).

WORKUP

后处理

  1. customwas removed by filtration
  2. washwashing with acetonitrile
  3. customthe filtrate evaporated to dryness under reduced pressure
  4. customPurification