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

HRID 629007ノート

反応式

HRID 629007 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-9238518658e34504a3ad54387e02e5fa
出典データセット
uspto-grants-2016_04
特許番号
US09315491B2

反応ノート

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