HRID133523

反应详情

EQUATION

反应方程式

HRID 133523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 70 mg (0.16 mmol) 3-acetyl-2-methyl-4-phenyl-5,8-dihydro-6H-9-thia-1,7-diaza-fluorene-7-carboxylic acid tert-butyl ester in 3 ml dicloromethane was added 0.2 ml trifluoroacetic acid. The mixture was stirred over night at RT, and then poured onto an aqueous solution of NaHCO3, and extracted three times with ethyl acetate. The combined organic phases were dried over sodium sulfate and concentrated in vacuo to afford 48 mg (94%) 1-(2-methyl-4-phenyl-5,6,7,8-tetrahydro-9-thia-1,7-diaza-fluoren-3-yl)-ethanone as a yellow solid. ES-MS m/e (%): 323 (M+H+, 100).

WORKUP

后处理

  1. extractionextracted three times with ethyl acetate
  2. dry with materialThe combined organic phases were dried over sodium sulfate
  3. concentrationconcentrated in vacuo