HRID1968903
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Trifluoroacetic acid (5 ml) was added to a cooled stirred solution of 6-[Benzyl-(1-methyl-1H-pyrazole-3-sulfonyl)-amino]-3,4-dihydro-1H-isoquinoline-2-carboxylic acid tert-butyl ester (391 mg, 0.80 mmol) in dichloromethane (20 ml). The mixture was allowed to warm to room temperature and stirred for 3 hrs then cooled and quenched with 2M NaOH until slightly basic. After diluting the reaction mixture with dichloromethane (100 ml) the organic phase was partitioned, dried over sodium sulfate and concentrated in vacuo to afford the title compound as a white solid (304 mg, 80% yield). HPLC retention time 2.97 min. Mass spectrum (ES+) m/z 383 (M+H).
WORKUP
后处理
- temperaturethen cooled
- customquenched with 2M NaOH until slightly basic
- additionAfter diluting the reaction mixture with dichloromethane (100 ml) the organic phase
- customwas partitioned
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo