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Hydrochloric Acid → 6-{4-[3-((R)-2-Methyl-pyrrolidin-1-yl)-propoxy]-phenyl}-4-pyridin-2-yl-4,5-dihydro-2H-pyridazin-3-one

HRID 2042639
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인쇄 미리보기

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HRID 2042639 반응식
C([O:3][C:4](=O)[CH:5]([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=1)[CH2:6][C:7]([C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][CH2:17][CH2:18][N:19]2[CH2:23][CH2:22][CH2:21][C@H:20]2[CH3:24])=[CH:11][CH:10]=1)=O)C.O.[NH2:33][NH2:34].Cl.CO>C(O)(=O)C>[CH3:24][C@@H:20]1[CH2:21][CH2:22][CH2:23][N:19]1[CH2:18][CH2:17][CH2:16][O:15][C:12]1[CH:13]=[CH:14][C:9]([C:7]2[CH2:6][CH:5]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=3)[C:4](=[O:3])[NH:33][N:34]=2)=[CH:10][CH:11]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 24654Hydrazine hydrate (1:1)HCID 596518864-{4-[3-((R)-2-Methyl-pyrrolidin-1-yl)-propoxy]-phenyl}-4-oxo-2-pyridin-2-yl-butyric acid ethyl ester

생성물 1

HCID 574028506-{4-[3-((R)-2-Methyl-pyrrolidin-1-yl)-propoxy]-phenyl}-4-pyridin-2-yl-4,5-dihydro-2H-pyridazin-3-one

시약·촉매·용매 1

HCID 176
Acetic Acid
용매

실험 절차

In a 50 mL round bottom flask, 4-{4-[3-((R)-2-methyl-pyrrolidin-1-yl)-propoxy]-phenyl}-4-oxo-2-pyridin-2-yl-butyric acid ethyl ester (950 mg, 1.84 mmol), and hydrazine monohydrate (204 μL, 4.2 mmol), in acetic acid (20 mL) was heated to reflux 14 h. The reaction was cooled and the solvent concentrated under vacuum. The slurry was partitioned between methylene chloride and NaHCO3 sol., extracted three times, and then dried over MgSO4. Purification with silica gel chromatography eluting with methylene chloride/methanol (95:5) produced 250 mg (33%). Ethereal HCl was added to a methanol solution to produce crystals. Mp 231-233° C. MS m/z 393 (M+H).

후처리

  1. temperatureto reflux 14 h
  2. temperatureThe reaction was cooled
  3. concentrationthe solvent concentrated under vacuum
  4. customThe slurry was partitioned between methylene chloride and NaHCO3 sol.
  5. extractionextracted three times
  6. dry with materialdried over MgSO4
  7. customPurification with silica gel chromatography
  8. washeluting with methylene chloride/methanol (95:5)
  9. customproduced 250 mg (33%)
  10. customto produce crystals

출처 및 근거

ORD 기록
ord-8154e67c43f048649847775bb94c069a
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586588B2

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