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Morpholine → HCID 86673505, 화합물

HRID 629016
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HRID 629016 반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([S:9][CH3:10])=[CH:4][N:3]=1.C([O-])([O-])=O.[Na+].[Na+].[NH:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1.CC(=O)OCC>CC(C)=O>[Cl:1][C:2]1[N:7]=[C:6]([N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[C:5]([S:9][CH3:10])=[CH:4][N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8083MorpholineHCID 8857Ethyl AcetateHCID 10340Sodium CarbonateHCID 2441072,4-Dichloro-5-(methylsulfanyl)pyrimidine

생성물 1

HCID 86673505HCID 86673505, 화합물수율 47.5%

시약·촉매·용매 1

HCID 180Acetone용매2회

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온도
0 °C

실험 절차

A solution of the 2,4-dichloro-5-(methylthio)pyrimidine (1.16 g, 6 mmole) in acetone (10 ml) at 0° C. containing Na2CO3 (1.1 eq, 6.6 mmole, 0.7 g) was treated dropwise with a solution of morpholine (1.0 eq, 6.6 mmole, 0.6 ml) in acetone (2 ml) and stirred for 1 hr at 0° C. TLC (EA:Hex=1:2, Rf=0.6) showed completion of the reaction to give two products. The acetone was removed in vacuo, the residue was partitioned between water and EA, and the organic layer was dried (MgSO4) and evaporated in vacuo. Column chromatography (EA/Hex=1/6) gave the product (700 mg, 47%).

후처리

  1. customcompletion of the reaction
  2. customto give two products
  3. customThe acetone was removed in vacuo
  4. customthe residue was partitioned between water and EA
  5. dry with materialthe organic layer was dried (MgSO4)
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-8c82c7cac02842708c1380b1bf947954
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09315491B2

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