Hydrochloric Acid → 2-Cycloheptylaminoethylfluorene

In dry tetrahydrofuran (30 ml) was dissolved 2-cycloheptylcarbamoylmethylfluorene (1.9 g) followed by dropwise addition of borane-methyl sulfide complex (1.8 ml) with ice-cooling. The mixture was then refluxed for 4 hrs, at the end of which time methanol (0.72 ml) was added with ice-cooling. The mixture was stirred at room temperature for 30 minutes, followed by addition of concentrated hydrochloric acid (1.8 ml) with ice-cooling. The mixture was refluxed again for 30 minutes. The reaction mixture was then cooled with ice and the resulting solid was recovered by filtration and washed with ether. The solid matter thus obtained was dissolved in chloroform and the solution was alkalinized with aqueous sodium hydroxide solution. The chloroform layer was taken and dried and the solvent was distilled off under reduced pressure to give 2-cycloheptylaminoethylfluorene (1.2 g).

1. additionfollowed by dropwise addition of borane-methyl sulfide complex (1.8 ml) with ice-
2. temperaturecooling
3. additionwas added with ice-
4. temperaturecooling
5. temperaturecooling
6. temperatureThe mixture was refluxed again for 30 minutes
7. temperatureThe reaction mixture was then cooled with ice
8. filtrationthe resulting solid was recovered by filtration
9. washwashed with ether
10. customThe solid matter thus obtained
11. customdried
12. distillationthe solvent was distilled off under reduced pressure

ORDレコード

ord-88fe0e8544dc45709b5cc8f6f38cc214

出典データセット

uspto-grants-1995_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05420348