Morpholine → HCID 58207334、化合物

HRID 1256290ノート

反応式

HRID 1256290 の反応式
Cl[C:2]1[N:7]2[N:8]=[CH:9][CH:10]=[C:6]2[N:5]=[C:4]([NH2:11])[CH:3]=1.[NH:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1.CN1C(=O)CCC1>O1CCOCC1>[O:15]1[CH2:16][CH2:17][N:12]([C:2]2[N:7]3[N:8]=[CH:9][CH:10]=[C:6]3[N:5]=[C:4]([NH2:11])[CH:3]=2)[CH2:13][CH2:14]1

参加物

5

反応物 3

HCID 8083MorpholineHCID 13387N-methyl-2-pyrrolidoneHCID 442513067-Chloropyrazolo[1,5-a]pyrimidin-5-amine

生成物 1

HCID 58207334HCID 58207334、化合物収率 38%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

7-Chloropyrazolo[1,5-a]pyrimidin-5-amine (1E, 10 g, 30 mmol) and morpholine were added to NMP (20 ml) and dioxane (80 ml). The mixture was heated to 100° C. and the resulting suspension was concentrated in vacuo to remove most of the dioxane. Brine was added and the mixture was extracted with EtOAc five times. Combined organics were washed with brine, dried over MgSO4, filtered and concentrated in vacuo. Trituration of the residue with Et2O gave the desired product 7-morpholinopyrazolo[1,5-a]pyrimidin-5-amine (9A, 5.0 g, 38%) as an off-white solid.

後処理

  1. concentrationthe resulting suspension was concentrated in vacuo
  2. customto remove most of the dioxane
  3. additionBrine was added
  4. extractionthe mixture was extracted with EtOAc five times
  5. washCombined organics were washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-3a9ee45bdec94c6c92b322f155cf28dc
出典データセット
uspto-grants-2013_06
特許番号
US08461163B2

反応ノート

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