Morpholine → 4-(2,6-Dichloro-5-methylsulfanyl-pyrimidin-4-yl)-morpholine

HRID 629007노트

반응식

HRID 629007 반응식
[Cl:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([S:9][CH3:10])=[C:4](Cl)[N:3]=1.[NH:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1>C1COCC1>[Cl:1][C:2]1[N:3]=[C:4]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[C:5]([S:9][CH3:10])=[C:6]([Cl:8])[N:7]=1

참가 물질

4

반응물 2

HCID 8083MorpholineHCID 122255442,4,6-Trichloro-5-methylsulfanyl-pyrimidine

생성물 1

HCID 866734944-(2,6-Dichloro-5-methylsulfanyl-pyrimidin-4-yl)-morpholine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 2,4,6-trichloro-5-methylsulfanyl-pyrimidine (4.0 g, 17.4 mmol.), morpholine (2.3 g, 26.1 mmol, 1.5 eq.) and THF (20 ml) was stirred at room temperature for 2.0 hr. The reaction mixture was dried and the solvent was evaporated. Thereafter, a 0.1 N HCl washing free morpholine was added to the solution. The solution was extracted with EA and the EA in the solution was removed by evaporation. A crude product was obtained. Purification of the crude by flash chromatography on silica gel (Hexane/EtOAc 6:1) gave a gray solid of 2.34 g (48.2%).

후처리

  1. customThe reaction mixture was dried
  2. customthe solvent was evaporated
  3. additionThereafter, a 0.1 N HCl washing free morpholine was added to the solution
  4. extractionThe solution was extracted with EA
  5. customthe EA in the solution was removed by evaporation

출처 및 근거

ORD 기록
ord-9238518658e34504a3ad54387e02e5fa
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315491B2

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