Morpholine → HCID 58207334, 화합물

HRID 1256290노트

반응식

HRID 1256290 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 58207334HCID 58207334, 화합물수율 38%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3a9ee45bdec94c6c92b322f155cf28dc
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461163B2

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