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2-Methyl-2-butene → HCID 58492412、化合物

HRID 2047995
ノート
印刷プレビュー

反応式

HRID 2047995 の反応式
[F:1][C:2]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH2:14][CH3:15])=[C:8]2[C:3]=1[C:4](=[O:28])[C:5]([C:20]1[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=1)=[CH:6][N:7]2[CH2:16][CH2:17][CH:18]=[O:19].Cl([O-])=[O:30].[Na+].CC(=CC)C.[Na].O.O.P(O)(O)(O)=O>O.ClCCl.C(O)(C)(C)C>[F:1][C:2]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH2:14][CH3:15])=[C:8]2[C:3]=1[C:4](=[O:28])[C:5]([C:20]1[CH:21]=[CH:22][C:23]([O:26][CH3:27])=[CH:24][CH:25]=1)=[CH:6][N:7]2[CH2:16][CH2:17][C:18]([OH:30])=[O:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 105532-Methyl-2-buteneHCID 23668197Sodium ChloriteHCID 584924253-[5-Fluoro-3-(4-methoxyphenyl)-4-oxo-8-propoxy-4H-quinolin-1-yl]propionaldehydeHCID 86658926CID 86658926

生成物 1

HCID 58492412HCID 58492412、化合物収率 68.1%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
2 回
HCID 6344Dichloromethane溶媒
HCID 6386tert-Butanol溶媒

実験手順

3-[5-Fluoro-3-(4-methoxyphenyl)-4-oxo-8-propoxy-4H-quinolin-1-yl]propionaldehyde (1.0 g, 2.61 mmol) was dissolved in water (10 ml), tert-butyl alcohol (20 ml) and dichloromethane (20 ml). Sodium chlorite (3.2 g, 35.4 mmol), 2-methyl-2-butene (19.86 gm, 283 mmol) and sodium-dihydrogenphosphate dihydrate (2 g, 2.61 mmol) were added to the resulting solution, and the solution was stirred at room temperature for 1 hour. Water was added to the reaction mixture, the mixture was extracted with dichloromethane, and then washed with water and dried over anhydrous sodium sulfate. The dried product was concentrated under reduced pressure. The residue was purified using silica gel column chromatography (dichloromethane:ethyl acetate=50:50→0:100). The purified product was concentrated to dryness under reduced pressure, giving a pale yellow powder of 3-[5-fluoro-3-(4-methoxyphenyl)-4-oxo-8-propoxy-4H-quinolin-1-yl]propionic acid (710 mg, yield: 68%).

後処理

  1. extractionthe mixture was extracted with dichloromethane
  2. washwashed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationThe dried product was concentrated under reduced pressure
  5. customThe residue was purified
  6. concentrationThe purified product was concentrated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-ac065cb7d47741638b233a953f184d8c
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08592593B2

反応ノート

読み込み中…

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