반응 #1539999

반응 방정식

diisopropylamine

2-propanol

(R)-2-bromoisovaleric acid

(R)-2-bromoisovaleric Acid

→

(R)-2-bromoisovaleric acid diisopropyl amine salt

수율 93.0%

용매

hexane

반응 조건

후처리

1. 1
   기타formed
2. 2
   기타to crystallize
3. 3
   여과The obtained crystals were filtered under a reduced pressure
4. 4
   세척the crystals were washed with 3 ml of a mixed solution of hexane/2-propanol=15/1 (V/V)
5. 5
   온도cooled to 5° C
6. 6
   기타The obtained crystals were dried under a reduced pressure

실험 절차

After continuously adding 1.68 g of diisopropylamine under a nitrogen atmosphere at 5° C. for 1 hour to a solution formed by adding 0.79 g of 2-propanol to 12.00 g of a hexane solution of (R)-2-bromoisovaleric acid obtained in Example 3 (containing 3.00 g of (R)-2-bromoisovaleric acid) to crystallize. They were successively stirred at 5° C. for 2 hours. The obtained crystals were filtered under a reduced pressure and then the crystals were washed with 3 ml of a mixed solution of hexane/2-propanol=15/1 (V/V) cooled to 5° C. The obtained crystals were dried under a reduced pressure to obtain 4.35 g of an (R)-2-bromoisovaleric acid diisopropyl amine salt (optical purity 99.1% ee, crystallization yield 93%, apparent purity 98.2%, impurity content 2-hydroxyisovaleric acid: not detected, bromine ingredient: 0.69%).

출처