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Sodium hydride → HCID 14148373, 화합물

HRID 247608
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HRID 247608 반응식
CC(C)([O-])C.[Na+].[H-].[Na+].[C:9]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([C:19]([CH3:22])([CH3:21])[CH3:20])[C:14]=1[OH:23])([CH3:12])([CH3:11])[CH3:10].[CH2:24]([N:28]1[C:32](=[O:33])[CH:31]=[CH:30][C:29]1=[O:34])[CH2:25][CH2:26][CH3:27]>C(O)(C)(C)C.O.C(O)(=O)C>[C:19]([C:15]1[CH:16]=[C:17]([CH:31]2[CH2:30][C:29](=[O:34])[N:28]([CH2:24][CH2:25][CH2:26][CH3:27])[C:32]2=[O:33])[CH:18]=[C:13]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:14]=1[OH:23])([CH3:22])([CH3:21])[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 24758Sodium hydrideHCID 314052,6-Di-tert-butylphenolHCID 239780N-ButylmaleimideHCID 23676156Sodium t-butoxide

생성물 1

HCID 14148373HCID 14148373, 화합물수율 12%

시약·촉매·용매 3

HCID 176Acetic Acid용매
HCID 962
Water
용매
HCID 6386tert-Butanol용매3회

실험 절차

To a solution of sodium tert-butoxide prepared from 2.40 g (0.1 mol) of sodium hydride and 135 ml of tert-butyl alcohol is added dropwise a solution of 20.63 g (0.1 mol) of 2,6-di-tert-butylphenol in 100 ml of tert-butyl alcohol. The reaction mixture is stirred at room temperature for 150 minutes and then to the resultant green solution is added dropwise over 120 minutes a solution of 15.31 g (0.1 mol.) of N-n-butylmaleimide in 50 ml of tert-butyl alcohol. The reaction mixture is stirred at room temperature overnight and is then mixed with 10 ml of glacial acetic acid. The reaction mixture is poured into 1.5 1 of water and the resultant mixture is extracted twice with chloroform. The organic extracts are combined and dried over anhydrous sodium sulfate. The solvent is removed in vacuo and the residue is purified by flash chromatography (3:1 heptane:toluene eluent) to give 4.25 g (12%) of a white solid: mp 109°-112° C.;

후처리

  1. stirringThe reaction mixture is stirred at room temperature overnight
  2. extractionthe resultant mixture is extracted twice with chloroform
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent is removed in vacuo
  5. customthe residue is purified by flash chromatography (3:1 heptane:toluene eluent)

출처 및 근거

ORD 기록
ord-0ba0710192d5404fb69e4eb32706a858
출처 데이터셋
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04709050

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