Triethylamine → HCID 22717680, 화합물

HRID 1582557

반응식

HRID 1582557 반응식
[CH2:1]([N:4]=[C:5]=[O:6])[CH:2]=[CH2:3].ON[C:9]([O:11]CC)=[O:10].C([N:16](CC)CC)C>CC(C)=O>[CH2:1]([N:4]1[C:9](=[O:10])[O:11][NH:16][C:5]1=[O:6])[CH:2]=[CH2:3]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 11510HydroxyurethaneHCID 15123Allyl isocyanate

생성물 1

HCID 22717680HCID 22717680, 화합물수율 158.9%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a 500 mL round-bottom flask were added acetone (300 mL), allyl isocyanate (12.0 g, 0.145 mol), N-hydroxyurethane (6.1 g, 0.058 mol) and triethylamine (11.7 g, 0.116 mol) respectively at room temperature under nitrogen with efficient stirring. The reaction mixture was allowed to stir at room temperature for 6 d. The solvent was removed under reduced pressure. The residue was suspended in 100 mL of 1N HCl, extracted with ethyl acetate (3×150 mL). The organic solution was washed with water, brine, dried over MgSO4 and concentrated to a clear yellow oil. The crude product was dried under high vacuum for 4 h to give the title compound as an oil (13.1 g) which was used in the next step without further purification.

후처리

  1. customThe solvent was removed under reduced pressure
  2. extractionextracted with ethyl acetate (3×150 mL)
  3. washThe organic solution was washed with water, brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated to a clear yellow oil
  6. dry with materialThe crude product was dried under high vacuum for 4 h

출처 및 근거

ORD 기록
ord-1c9694b018d84fe89c2602412811fbc3
출처 데이터셋
uspto-grants-2004_05
특허 번호
US06737383B1

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