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

HRID 3077

반응식

HRID 3077 반응식
[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]

참가 물질

5

반응물 2

HCID 244Benzyl AlcoholHCID 354092-Isocyanatoethyl methacrylate

생성물 1

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

시약·촉매·용매 2

HCID 9809426Di-n-butyldilauryltin촉매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-921b325d103d4c73b989008641f1fd3d
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733707

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