반응 #51266

반응 방정식

ammonium chloride

n-butyllithium

4,4-dimethyl-8-iodochroman

DMF

→

4,4-dimethylchroman-8-carbaldehyde

용매

THF

반응 조건

후처리

1. 1
   기타to return to room temperature
2. 2
   추출extracted with ethyl ether
3. 3
   기타the organic phase is separated
4. 4
   건조dried over magnesium sulphate
5. 5
   기타evaporated
6. 6
   기타10.40 g (100%) of the expected compound are collected in the form of a yellow oil

실험 절차

14.40 g (50.0 mmol) of 4,4-dimethyl-8-iodochroman and 50 ml of THF are introduced into a three-necked flask under a stream of nitrogen. 22 ml (55.0 mmol) of n-butyllithium (2.5M in hexane) are added dropwise at −78° C., the reaction mixture is stirred for 30 minutes, then 4.2 ml (55.0 mmol) of DMF are added and the mixture is allowed to return to room temperature. The reaction mixture is poured onto an aqueous ammonium chloride solution and extracted with ethyl ether and the organic phase is separated by settling, dried over magnesium sulphate and evaporated. 10.40 g (100%) of the expected compound are collected in the form of a yellow oil.

출처