반응 #1929067

반응 방정식

compound

1-Amino-4,4-difluorocyclohexanecarboxylic acid

methanol

thionyl chloride

→

Methyl 1-amino-4,4-difluorocyclohexanecarboxylate hydrochloride

반응 조건

후처리

1. 1
   온도The mixture was then cooled to 5° C.
2. 2
   여과the precipitate was filtered off with suction
3. 3
   농축The solution was concentrated
4. 4
   기타a rotary evaporator
5. 5
   기타the residue was crystallized

실험 절차

Under argon, 4.30 g of the compound from Example 3A were initially charged in 100 ml of methanol at 0 to 5° C. 10 ml of thionyl chloride were added dropwise, and the mixture was stirred at 0° C. for 30 minutes and at 70° C. for 24 h. The mixture was then cooled to 5° C. and the precipitate was filtered off with suction. The solution was concentrated using a rotary evaporator and the residue was crystallized using methyl tert-butyl ether. This gave 5.20 g (quantitative, still contains salts) of the title compound.

출처