반응 #339057

반응 방정식

2-((R)-6,8-Dichloro-2-cyclopropyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenylamine

2-chloroethyl chloroformate

→

desired product

수율 132.1%

3-[2-((R)-6,8-Dichloro-2-cyclopropyl-1,2,3,4-tetrahydroisoquinolin-4-yl)-phenyl]oxazolidin-2-one

수율 132.1%

용매

THF

반응 조건

후처리

1. 1
   workup.STIRRINGAfter stirring at room temperature for 3 h
2. 2
   workup.WAITthe mixture was left
3. 3
   기타The solvent was then removed
4. 4
   기타the residue purified by means of preparative HPLC
5. 5
   기타the acetonitrile was removed on a rotary evaporator
6. 6
   추출extracted three times with ethyl acetate
7. 7
   건조After the combined ethyl acetate phases had been dried over magnesium sulfate, they
8. 8
   여과were filtered
9. 9
   농축concentrated to dryness

실험 절차

2-((R)-6,8-Dichloro-2-cyclopropyl-1,2,3,4-tetrahydroisoquinolin-4-yl)phenylamine (400 mg) was dissolved in absolute THF (25 ml), and 2-chloroethyl chloroformate (102 mg) was added with stirring. After stirring at room temperature for 3 h, the mixture was left to stand overnight. The solvent was then removed and the residue purified by means of preparative HPLC. The fractions comprising product were combined, the acetonitrile was removed on a rotary evaporator, and the aqueous residue was neutralized with saturated sodium hydrogencarbonate solution and extracted three times with ethyl acetate. After the combined ethyl acetate phases had been dried over magnesium sulfate, they were filtered and concentrated to dryness. 380 mg of the desired product were obtained.

출처