Cyclohexylamine → 1-Cyclohexyl-3-methacryloxyethyl urea

HRID 265720

反応式

HRID 265720 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 542409741-Cyclohexyl-3-methacryloxyethyl urea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f1a8535af413410c83dc3b564b346c4e
出典データセット
uspto-grants-1997_07
特許番号
US05648515

関連ノート

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