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

HRID 1775376
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HRID 1775376 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 57096144,4,4-Trifluorocrotonic acid용매

실험 절차

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]+.

후처리

  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)

출처 및 근거

ORD 기록
ord-f933a801f41a47999eee4777ae947b5f
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09260441B2

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