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Water → 4-[4-(3-Chloro-propoxy)-phenyl]-4-oxo-2-pyridin-2-yl-butyric acid ethyl ester

HRID 2042637
ノート
印刷プレビュー

反応式

HRID 2042637 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].[H-].[Na+].Br[CH2:16][C:17]([C:19]1[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][CH2:28][Cl:29])=[CH:21][CH:20]=1)=[O:18].O>CN(C)C=O>[CH2:11]([O:10][C:8](=[O:9])[CH:7]([C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=1)[CH2:16][C:17]([C:19]1[CH:24]=[CH:23][C:22]([O:25][CH2:26][CH2:27][CH2:28][Cl:29])=[CH:21][CH:20]=1)=[O:18])[CH3:12]
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 962WaterHCID 24758Sodium hydrideHCID 75960Ethyl 2-pyridylacetateHCID 140970932-Bromo-1-[4-(3-chloro-propoxy)-phenyl]-ethanone

生成物 1

HCID 596520644-[4-(3-Chloro-propoxy)-phenyl]-4-oxo-2-pyridin-2-yl-butyric acid ethyl ester

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒
2 回

実験手順

In a 500 mL round bottom flask ethyl 2-pyridylacetate (2.0 g, 12.1 mmol), and 60% sodium hydride (508 mg, 12.7 mmol) in dimethylformamide (50 mL) was stirred 1 h. 2-Bromo-1-[4-(3-chloro-propoxy)-phenyl]-ethanone (3.53 g, 12.1 mmol) was then added in dimethylformamide (50 mL) via dropping funnel. The reaction was stirred 14 h. Water (300 mL) was added and the organics were extracted three times with ethyl acetate, and then dried over MgSO4. Purification with silica gel chromatography eluting with hexanes/ethyl acetate (3:1) produced 2.8 g (62%). MS m/z 376 (M+H).

後処理

  1. extractionthe organics were extracted three times with ethyl acetate
  2. dry with materialdried over MgSO4
  3. customPurification with silica gel chromatography
  4. washeluting with hexanes/ethyl acetate (3:1)
  5. customproduced 2.8 g (62%)

出典と根拠

ORDレコード
ord-b046712e335048a29786ae3387708d67
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

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