반응 #1540001

반응 방정식

diisopropylamine

(R)-2-bromoisovaleric acid

→

(R)-2-bromoisovaleric acid diisopropylamine salt

수율 80.0%

용매

methyl t-butyl ether

반응 조건

후처리

1. 1
   기타obtained in Comparative Example 2
2. 2
   workup.ADDITIONwas continuously added at −4° C. for 12 min
3. 3
   기타to crystallize
4. 4
   기타Obtained crystals
5. 5
   여과were filtered under a reduced pressure
6. 6
   세척washed with 30 ml of methyl t-butyl ether
7. 7
   기타Obtained crystals
8. 8
   기타were dried under a reduced pressure

실험 절차

After continuously adding 16 ml of diisopropylamine to 128.9 g of a methyl t-butyl ether solution of (R)-2-bromoisovaleric acid obtained in Comparative Example 2 was continuously added at −4° C. for 12 min to crystallize, they were stirred successively at 0° C. for 1 hour. Obtained crystals were filtered under a reduced pressure, and then washed with 30 ml of methyl t-butyl ether. Obtained crystals were dried under a reduced pressure to obtain 27.81 g of (R)-2-bromoisovaleric acid diisopropylamine salt (optical purity 98.1% ee, crystallization yield 80%, apparent purity 92.5%, impurity content 2-hydroxy isovaleric acid; 0.31%, bromine content: 4.58%).

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