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Sodium Hydroxide → 5-Fluoro-3-piperazino benzofuran

HRID 2241973
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HRID 2241973 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

HCID 214718555-Fluoro-3-piperazino benzofuran수율 35.4%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ba9a9fff95924b1099635ac2aea0ca82
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07671056B2

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