Dichloromethane → 4-Methyl-2-(piperazin-1-yl)pyrimidine dihydrochloride

HRID 1775324노트

반응식

HRID 1775324 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([N:8]2[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9]2)[N:3]=1.C(Cl)[Cl:22]>FC(F)(F)C(O)=O>[ClH:22].[ClH:22].[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([N:8]2[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]2)[N:3]=1

참가 물질

4

반응물 2

HCID 6344DichloromethaneHCID 15132529tert-Butyl 4-(4-methylpyrimidin-2-yl)piperazine-1-carboxylate

생성물 1

HCID 183649784-Methyl-2-(piperazin-1-yl)pyrimidine dihydrochloride수율 71%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

The product from the previous step (tert-butyl 4-(4-methylpyrimidin-2-yl)piperazine-1-carboxylate) was dissolved in a one-to-one mixture of trifluoroacetic acid and DCM (8 ml) and stirred at room temperature for three hours. The volatiles were removed under reduced pressure, the residue was dissolved in DCM and evaporated. The residue was dissolved in THF (10 ml), HCl in dioxane (4N, 2 ml) was added and the resulting precipitate was collected by repeated centrifugation, dekantation and washing with THF to yield 107 mg of a solid (0.30 mmol, 71%). MS (APCI) m/z=179.1 [M+1]+.

후처리

  1. customThe volatiles were removed under reduced pressure
  2. dissolutionthe residue was dissolved in DCM
  3. customevaporated
  4. dissolutionThe residue was dissolved in THF (10 ml)
  5. additionHCl in dioxane (4N, 2 ml) was added
  6. customthe resulting precipitate was collected
  7. washwashing with THF

출처 및 근거

ORD 기록
ord-157bd86215b644048653cf862e9d567b
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09260441B2

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