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Sodium Hydroxide → 5-Fluoro-3-piperazino benzofuran

HRID 2241973
ノート
印刷プレビュー

反応式

HRID 2241973 の反応式
C(OC([N:6]1[CH2:11][CH2:10][N:9]([C:12]2[C:16]3[CH:17]=[C:18]([F:21])[CH:19]=[CH:20][C:15]=3[O:14][CH:13]=2)[CH2:8][CH2:7]1)=O)C.[OH-].[Na+]>C(O)C>[F:21][C:18]1[CH:19]=[CH:20][C:15]2[O:14][CH:13]=[C:12]([N:9]3[CH2:8][CH2:7][NH:6][CH2:11][CH2:10]3)[C:16]=2[CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 592048394-(5-Fluorobenzofuran-3-yl)-piperazine-1-carboxylic acid ethyl ester

生成物 1

HCID 214718555-Fluoro-3-piperazino benzofuran収率 35.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

4-(5-fluorobenzofuran-3-yl)-piperazine-1-carboxylic acid ethyl ester (Step 1, 3 g) was dissolved in 95% ethanol and 3N aqueous sodium hydroxide (25 mL) was added. The reaction mixture was stirred at reflux for 24 hours. The mixture was then cooled to room temperature, concentrated on a rotary evaporator to remove the ethanol and extracted with chloroform. The combined organic layers were washed with brine, dried over anhydrous MgSO4, filtered and concentrated on a rotary evaporator. The desired product (0.8 g) was obtained as a brown oil and was used without further purification; MS (ES) m/z (relative intensity): 221 (M+H)+ (100).

後処理

  1. temperatureat reflux for 24 hours
  2. concentrationconcentrated on a rotary evaporator
  3. customto remove the ethanol
  4. extractionextracted with chloroform
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over anhydrous MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated on a rotary evaporator

出典と根拠

ORDレコード
ord-ba9a9fff95924b1099635ac2aea0ca82
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07671056B2

反応ノート

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