Реакция #1929067

Уравнение реакции

compound

1-Amino-4,4-difluorocyclohexanecarboxylic acid

methanol

thionyl chloride

→

Methyl 1-amino-4,4-difluorocyclohexanecarboxylate hydrochloride

Условия реакции

Обработка

1. 1
   ТемператураThe mixture was then cooled to 5° C.
2. 2
   Фильтрацияthe precipitate was filtered off with suction
3. 3
   КонцентрированиеThe solution was concentrated
4. 4
   Другоеa rotary evaporator
5. 5
   Другоеthe residue was crystallized

Методика

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.

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