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Dichloromethane → 1-(4-Ethoxy-6-methyl-2-pyridyl)piperazine hydrochloride

HRID 1775376
ノート
印刷プレビュー

反応式

HRID 1775376 の反応式
[CH2:1]([O:3][C:4]1[CH:9]=[C:8]([CH3:10])[N:7]=[C:6]([N:11]2[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][CH2:12]2)[CH:5]=1)[CH3:2].C(Cl)[Cl:25]>FC(F)(F)/C=C/C(O)=O>[ClH:25].[CH2:1]([O:3][C:4]1[CH:9]=[C:8]([CH3:10])[N:7]=[C:6]([N:11]2[CH2:12][CH2:13][NH:14][CH2:15][CH2:16]2)[CH:5]=1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6344DichloromethaneHCID 131734740tert-Butyl 4-(4-ethoxy-6-methyl-2-pyridyl)piperazine-1-carboxylate

生成物 1

HCID 898258231-(4-Ethoxy-6-methyl-2-pyridyl)piperazine hydrochloride

試薬・触媒・溶媒 1

HCID 57096144,4,4-Trifluorocrotonic acid溶媒

実験手順

tert-Butyl 4-(4-ethoxy-6-methyl-2-pyridyl)piperazine-1-carboxylate (141 mg, 0.44 mmol) was dissolved in a mixture of DCM (5 ml) and trifluorocrotonic acid (5 ml) and left standing at room temperature for two hours. The mixture was concentrated under reduced pressure, the residue was dissolved in THF, evaporated again, dissolved again in THF. Hydrochloric acid (4N in dioxane) was added to precipitate the product, which was collected by filtration, washed with diethylether and dried under reduced pressure to give 115 mg (quantitative) MS (multi-mode) m/z=222.2 [M+H]+.

後処理

  1. waitleft
  2. concentrationThe mixture was concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in THF
  4. customevaporated again
  5. dissolutiondissolved again in THF
  6. additionHydrochloric acid (4N in dioxane) was added
  7. customto precipitate the product, which
  8. filtrationwas collected by filtration
  9. washwashed with diethylether
  10. customdried under reduced pressure
  11. customto give 115 mg (quantitative)

出典と根拠

ORDレコード
ord-f933a801f41a47999eee4777ae947b5f
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09260441B2

反応ノート

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