Benzyl Alcohol → 2-{[(Benzyloxy)carbonyl]amino}ethyl 2-methylprop-2-enoate

HRID 3077

反応式

HRID 3077 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].[CH2:12]([OH:19])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>O1CCOCC1.C([O-])(=O)CCCCCCCCCCC.C([O-])(=O)CCCCCCCCCCC.C([Sn+2]CCCC)CCC>[C:1]([O:6][CH2:7][CH2:8][NH:9][C:10]([O:19][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[O:11])(=[O:5])[C:2]([CH3:4])=[CH2:3]

参加物

5

反応物 2

HCID 244Benzyl AlcoholHCID 354092-Isocyanatoethyl methacrylate

生成物 1

HCID 138396362-{[(Benzyloxy)carbonyl]amino}ethyl 2-methylprop-2-enoate収率 80.6%

試薬・触媒・溶媒 2

HCID 9809426Di-n-butyldilauryltin触媒HCID 312751,4-Dioxane溶媒

実験手順

77.5 g of methacryloyloxyethyl isocyanate (Karenzu MOI, available from Showa Denko K.K.) and 60 g of benzyl alcohol were dissolved in 260 g of dioxane. To the solution were then added 5 drops of di-n-butyltin dilaurate. The reaction mixture was then allowed to undergo reaction at a temperature of 65° C. for 3 hours. The dioxane and excess benzyl alcohol were then distilled off under reduced pressure. The residue was poured into water, extracted with ethyl acetate, and then dried. The solvent was then distilled off to obtain 106 g of benzyloxycarbonylaminoethyl methacrylate in the form of colorless oil.

後処理

  1. customreaction at a temperature of 65° C. for 3 hours
  2. distillationThe dioxane and excess benzyl alcohol were then distilled off under reduced pressure
  3. additionThe residue was poured into water
  4. extractionextracted with ethyl acetate
  5. customdried
  6. distillationThe solvent was then distilled off

出典と根拠

ORDレコード
ord-921b325d103d4c73b989008641f1fd3d
出典データセット
uspto-grants-1998_03
特許番号
US05733707

関連ノート

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