Methyl iodide → 2-iodo-9,9-dimethyl-9H-fluorene

温度

25 °C

20 parts of 2-iodofluorene was dissolved in a mixed solution of 114 parts of dimethyl sulfoxide (DMSO) and 23 parts of tetrahydrofuran (THF), and the thus obtained mixture was then stirred at 25° C. for 10 minutes. Thereafter, while stirring, 8.7 parts of potassium-tert-butoxide was added to the mixture. Twenty minutes later, 13.2 parts of methyl iodide was added to the mixture, and further twenty minutes later, 8.7 parts of potassium-tert-butoxide was added thereto. Further, twenty minutes later, 13.2 parts of methyl iodide was added thereto, and the obtained mixture was then stirred at 25° C. for 2 hours. After completion of the stirring, the THF was distilled away from the reaction solution, and it was then extracted with toluene-water. The toluene phase was dried over magnesium sulfate, and the toluene was then distilled away, thereby obtaining a brown tarry solid. This brown tarry solid was separated and purified by column chromatography (hexane-ethyl acetate) to obtain 21 parts of 9,9-dimethyl-2-iodofluorene in the form of a colorless crystal.

1. stirringThereafter, while stirring
2. stirringthe obtained mixture was then stirred at 25° C. for 2 hours
3. distillationAfter completion of the stirring, the THF was distilled away from the reaction solution, and it
4. extractionwas then extracted with toluene-water
5. dry with materialThe toluene phase was dried over magnesium sulfate
6. distillationthe toluene was then distilled away
7. customobtaining a brown tarry solid
8. customThis brown tarry solid was separated
9. custompurified by column chromatography (hexane-ethyl acetate)

ORDレコード

ord-f80058a1a4d944119bb48b99cee66038

出典データセット

uspto-grants-2014_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08735720B2