N-Phenylmaleimide → HCID 14148372, 화합물

HRID 247614

반응식

HRID 247614 반응식
[H-].[Na+].[C:3]([C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([C:13]([CH3:16])([CH3:15])[CH3:14])[C:8]=1[OH:17])([CH3:6])([CH3:5])[CH3:4].[C:18]1([N:24]2[C:28](=[O:29])[CH:27]=[CH:26][C:25]2=[O:30])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>O1CCCC1>[C:13]([C:9]1[CH:10]=[C:11]([CH:27]2[CH2:26][C:25](=[O:30])[N:24]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[C:28]2=[O:29])[CH:12]=[C:7]([C:3]([CH3:6])([CH3:5])[CH3:4])[C:8]=1[OH:17])([CH3:16])([CH3:15])[CH3:14]

참가 물질

5

반응물 3

HCID 13662N-PhenylmaleimideHCID 24758Sodium hydrideHCID 314052,6-Di-tert-butylphenol

생성물 1

HCID 14148372HCID 14148372, 화합물수율 2.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

This compound is prepared by the procedure of Example 1 from 2.40 g (0.1 mol) of sodium hydride, 20.63 g (0.1 mol) of 2,6-di-tert-butylphenol, and 17.32 g (0.1 mol) of N-phenylmaleimide in tetrahydrofuran. The reaction mixture is concentrated in vacuo and the residue is dissolved in 150 ml of toluene. The toluene solution is extracted sequentially with 1M sodium hydroxide (2×100 ml) and water (2×50 ml). The organic phase is dried over anhydrous sodium sulfate and then the solvent is removed in vacuo. The residue is triturated with petroleum ether to give 0.78 g (2%) of white crystals: mp 204° C.

후처리

  1. concentrationThe reaction mixture is concentrated in vacuo
  2. dissolutionthe residue is dissolved in 150 ml of toluene
  3. extractionThe toluene solution is extracted sequentially with 1M sodium hydroxide (2×100 ml) and water (2×50 ml)
  4. dry with materialThe organic phase is dried over anhydrous sodium sulfate
  5. customthe solvent is removed in vacuo
  6. customThe residue is triturated with petroleum ether

출처 및 근거

ORD 기록
ord-c2d334ca504d491ba5ca09fb968575eb
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04709050

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