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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
ノート
印刷プレビュー

反応式

HRID 2042639 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176
Acetic Acid
溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-8154e67c43f048649847775bb94c069a
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08586588B2

反応ノート

読み込み中…

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