Water → HCID 13671565, 화합물

HRID 745206

반응식

HRID 745206 반응식
[CH:1]12[C:9](=[O:10])[NH:8][C:7](=[O:11])[CH:2]1[CH2:3][CH2:4][CH2:5][CH2:6]2.[H-].[Na+].[CH2:14](Br)[CH2:15][CH2:16][CH2:17][Br:18].O>CN(C)C=O>[Br:18][CH2:17][CH2:16][CH2:15][CH2:14][N:8]1[C:7](=[O:11])[CH:2]2[CH2:3][CH2:4][CH2:5][CH2:6][CH:1]2[C:9]1=[O:10]

참가 물질

6

반응물 4

HCID 962WaterHCID 80561,4-DibromobutaneHCID 24758Sodium hydrideHCID 735591H-Isoindole-1,3(2H)-dione, hexahydro-

생성물 1

HCID 13671565HCID 13671565, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of cyclohexane-1,2-dicarboximide (10 g; 65.3 mmol) in anhydrous dimethylformamide (50 ml), there was added 60% sodium hydride (2.6 g; 68.5 mmol) under nitrogen at room temperature, and the resultant mixture was stirred at the same temperature for 3 hours. Tetramethylene bromide (70.5 g; 0.327 mol) was added thereto, and the mixture was stirred for 3 hours. After completion of the reaction, the resultant mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with water twice and with a saturated sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate, and the solvent and excessive tetramethylene bromide were removed by evaporation to give N-(4-bromobutyl)cyclohexane-1,2-dicarboximide. IR νmaxFilm (cm-1): 1770, 1700.

후처리

  1. customAfter completion of the reaction
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water twice
  4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  5. customthe solvent and excessive tetramethylene bromide were removed by evaporation

출처 및 근거

ORD 기록
ord-76bce555f5aa4f76be20fccc37284434
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04598078

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