Cyclohexylamine → 1-Cyclohexyl-3-methacryloxyethyl urea

HRID 234081

반응식

HRID 234081 반응식
[C:1]([O:6][CH2:7][CH2:8][N:9]=[C:10]=[O:11])(=[O:5])[C:2]([CH3:4])=[CH2:3].C1C=C2C=CC(O)=C(C3C4C(=CC=CC=4)C=CC=3O)C2=CC=1.[CH:34]1([NH2:40])[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1.C([O-])(=O)CCCCCCCCCCC.C([O-])(=O)CCCCCCCCCCC.C([Sn+2]CCCC)CCC>C(Cl)Cl>[CH:34]1([NH:40][C:10]([NH:9][CH2:8][CH2:7][O:6][C:1](=[O:5])[C:2]([CH3:4])=[CH2:3])=[O:11])[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]1

참가 물질

6

반응물 4

HCID 7965CyclohexylamineHCID 11762BinolHCID 354092-Isocyanatoethyl methacrylateHCID 9809426Di-n-butyldilauryltin

생성물 1

HCID 542409741-Cyclohexyl-3-methacryloxyethyl urea

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A 3-neck, 250-mL round bottom flask equipped with a reflux condenser was charged with isocyanatoethyl methacrylate (7.79 g), 1,1'-bi-2-naphthol (1.3 mg) and 50 mL of methylene chloride. While stirring, cyclohexylamine (5.24 g) and dibutyltin dilaurate (52.3 mg) in 50 mL of methylene chloride were added over a 15 minute period. The reaction mixture was kept stirred for an additional 30 minutes. The solution was filtered and evaporated to dryness to recover the product. The product was characterized by H-NMR, 0.72-2.10 ppm (m, 1H), 1.90 ppm (s, 3H), 3.45 ppm (t, 2H), 3.50 ppm (hidden, 1H), 4.18 ppm (t, 2H), 5.12 ppm (s, 1H), 5.26 ppm (s, 1H), 5.52 ppm (s, 1H), 6.10 ppm (s, 1H).

후처리

  1. customA 3-neck, 250-mL round bottom flask equipped with a reflux condenser
  2. stirringThe reaction mixture was kept stirred for an additional 30 minutes
  3. filtrationThe solution was filtered
  4. customevaporated to dryness
  5. customto recover the product

출처 및 근거

ORD 기록
ord-e2ada60320fa467180888be54a6e0185
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05594085

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