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Dimethylformamide → HCID 53957464, 화합물

HRID 1756772
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HRID 1756772 반응식
[CH:1]([C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([CH:12]([CH3:14])[CH3:13])[C:5]=1[CH2:6]Cl)([CH3:3])[CH3:2].[C:15]1(=[O:25])[NH:19][C:18](=[O:20])[C:17]2=[CH:21][CH:22]=[CH:23][CH:24]=[C:16]12.[K].CN(C)C=O>O>[CH:1]([C:4]1[CH:11]=[CH:10][CH:9]=[C:8]([CH:12]([CH3:14])[CH3:13])[C:5]=1[CH2:6][N:19]1[C:18](=[O:20])[C:17]2=[CH:21][CH:22]=[CH:23][CH:24]=[C:16]2[C:15]1=[O:25])([CH3:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 24194345Phthalimide potassium saltHCID 54108381HCID 54108381, 화합물

생성물 1

HCID 53957464HCID 53957464, 화합물수율 71.4%

시약·촉매·용매 1

HCID 962Water용매

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온도
70 °C

실험 절차

A mixture of 0.92 g (4.4 mmol) of 2, 6-diisopropylbenzyl chloride, 0.97 g (5.24 mmol) of potassium phthalimide and 8 ml of N, N-dimethylformamide was stirred at 70° C. for 1.5 hours. After cooling, the reaction mixture was mixed with water and extracted with ethyl acetate. The extract was washed with saturated saline, dried over anhydrous magnesium sulfate and the solvent evaporated in vacuo. The residue was mixed with 15 ml of hexane and 2 ml of ethyl acetate, stirred at room temperature, and the precipitated crystals were filtered to give 1.01 g of N-(2, 6-diisopropylbenzyl)-phthalimide.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with saturated saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent evaporated in vacuo
  6. additionThe residue was mixed with 15 ml of hexane and 2 ml of ethyl acetate
  7. stirringstirred at room temperature
  8. filtrationthe precipitated crystals were filtered

출처 및 근거

ORD 기록
ord-16c9a2ebf6844efe82e37f642057af9b
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05442060

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