Iodoethane → 1,3-Dibromo-2-ethylbenzene

Temperatur

-78 °C

A three necked round-bottom flask was purged with argon and then filled with dry THF (1.2 l), 1,3-dibromo benzene (121 g, 0.514 mol) and ethyl iodide (95.4 g, 0.611 mol). The mixture was cooled to −78° C. and LDA (64.2 g, 0.697 mol) (2 M in THF/n-heptane/ethyl benzene) was added slowly in a way that the temperature did not rise above −65° C. After stirring for 2.75 h the reaction was poured onto 1 l sat. aq. NH4Cl solution and stirred vigorously for 20 min. Two times extraction with DCM yielded colorless oil (167 g) which was used in the next step without further purification.

1. customA three necked round-bottom flask was purged with argon
2. customdid not rise above −65° C
3. stirringstirred vigorously for 20 min
4. extractionTwo times extraction with DCM yielded colorless oil (167 g) which
5. customwas used in the next step without further purification

ORD-Eintrag

ord-07d968876b81431686c441504a41308c

Quelldatensatz

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08835653B2