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Hydrochloric Acid → HCID 178511526, 화합물

HRID 1600685
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HRID 1600685 반응식
C(OC(=O)[NH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([CH2:14][C:15](=[O:28])[N:16]2[CH2:21][CH2:20][N:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:18][CH2:17]2)[CH2:10][CH2:9]1)(C)(C)C.Cl.O1CCOCC1.[OH-].[Na+]>CO>[O:28]=[C:15]([N:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:18][CH2:17]1)[CH2:14][C@H:11]1[CH2:10][CH2:9][C@H:8]([NH2:7])[CH2:13][CH2:12]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 312751,4-DioxaneHCID 178453926HCID 178453926, 화합물

생성물 1

HCID 178511526HCID 178511526, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Trans-{4-[2-oxo-2-(4-phenyl-piperazin-1-yl)-ethyl]-cylohexyl}-carbamic acid tert-butyl ester (18.1 g, 0.045 mol) was taken up in MeOH (275 mL) and treated with 4 M HCl in dioxane (56 mL, 0.224 mol) and allowed to stand 22 hours. Concentration to dryness yielded a solid which was treated with 2N NaOH (175 mL) and extracted with CH2Cl2. The extracts were washed with water, brine, and dried (Na2SO4). After evaporation of the solvent, the residue was crystallized in Et2O yielding trans-{4-[2-oxo-2-(4-phenyl-piperazin-1-yl)-ethyl]-cyclohexyl}-amine as a white solid, 11.2 g (83%); mp 90-93° C.

후처리

  1. concentrationConcentration to dryness
  2. customyielded a solid which
  3. extractionextracted with CH2Cl2
  4. washThe extracts were washed with water, brine
  5. dry with materialdried (Na2SO4)
  6. customAfter evaporation of the solvent
  7. customthe residue was crystallized in Et2O

출처 및 근거

ORD 기록
ord-dc45d9192fa34acfb52568dc8719bf74
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05977110

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