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

HRID 1775324ノート

反応式

HRID 1775324 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-157bd86215b644048653cf862e9d567b
出典データセット
uspto-grants-2016_02
特許番号
US09260441B2

反応ノート

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