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

HRID 573989노트

반응식

HRID 573989 반응식
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[Cl:7][C:8]1[N:13]=[C:12](Cl)[C:11]([F:15])=[C:10]([Cl:16])[N:9]=1>C(O)C>[Cl:7][C:8]1[N:13]=[C:12]([N:1]2[CH2:6][CH2:5][O:4][CH2:3][CH2:2]2)[C:11]([F:15])=[C:10]([Cl:16])[N:9]=1

참가 물질

4

반응물 2

HCID 8083MorpholineHCID 133889932,4,6-Trichloro-5-fluoropyrimidine

생성물 1

HCID 866441264-(2,6-Dichloro-5-fluoropyrimidin-4-yl)morpholine수율 53.1%

시약·촉매·용매 1

HCID 702Ethanol용매2회

반응 조건

온도
-20 °C

실험 절차

A solution of morpholine (1.5 mL, 17.05 mmol) in ethanol (25 mL) was added to a cooled (−20° C.) solution of 2,4,6-trichloro-5-fluoropyrimidine (3.00 g, 14.93 mmol) in ethanol (150 mL) and the resulting mixture was stirred at −20° C. for 30 minutes and at ambient temperature for 3 hours. The solvent was evaporated under reduced pressure and the residue was partitioned between water and methylene chloride. The organic layer was separated, dried and the solvent evaporated under reduced pressure. The resulting white solid was triturated with ethanol, then filtered and dried to give the title compound (2.0 g, 53%).

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was partitioned between water and methylene chloride
  3. customThe organic layer was separated
  4. customdried
  5. customthe solvent evaporated under reduced pressure
  6. customThe resulting white solid was triturated with ethanol
  7. filtrationfiltered
  8. customdried

출처 및 근거

ORD 기록
ord-64f952acd6d84900bfc76b6b55c02925
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034311B2

반응 노트

불러오는 중…