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

HRID 573989ノート

反応式

HRID 573989 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

反応条件

温度
-20 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-64f952acd6d84900bfc76b6b55c02925
出典データセット
uspto-grants-2015_05
特許番号
US09034311B2

反応ノート

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