Ethylmorpholine → N-((Phenylmethoxy)carbonyl)glycine ethyl ester

HRID 2295709노트

반응식

HRID 2295709 반응식
[NH2:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].Cl.C(N1CCOCC1)C.CP(OP(CC)(C)=O)(CC)=O.[C:28](NCC(O)=O)([O:30][CH2:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)=[O:29]>CN(C=O)C>[CH2:6]([O:5][C:3](=[O:4])[CH2:2][NH:1][C:28]([O:30][CH2:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)=[O:29])[CH3:7]

참가 물질

6

반응물 4

HCID 7525EthylmorpholineHCID 14349BenzyloxycarbonylglycineHCID 103894Phosphinic acid, P-ethyl-P-methyl-, P,P'-anhydrideHCID 2723640Glycine ethyl ester, hydrochloride

생성물 1

HCID 14366N-((Phenylmethoxy)carbonyl)glycine ethyl ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

At 0° C., 7.0 g (0.05 mol) of H-Gly-OC2H5.HCl, 15 ml of N-ethyl morpholine and 20 g of methylethylphosphinic acid anhydride were added successively to a solution of 10.5 g (0.05 mol) of carbobenzoxy-glycine in 20 ml DMF, while stirring and cooling thoroughly. The mixture was brought to room temperature, while stirring. After 16 hours of standing at room temperature the solvent was distilled off in vacuo, and the residue was dissolved in a mixture of 200 ml of ethyl acetate and 100 ml of a 5% potassium bisulfate solution. The ethyl acetate solution was washed twice with 100 ml each of saturated sodium bicarbonate solution, dried over sodium sulfate and evaporated in vacuo.

후처리

  1. temperaturecooling thoroughly
  2. customwas brought to room temperature
  3. stirringwhile stirring
  4. distillationthe solvent was distilled off in vacuo
  5. dissolutionthe residue was dissolved in a mixture of 200 ml of ethyl acetate and 100 ml of a 5% potassium bisulfate solution
  6. washThe ethyl acetate solution was washed twice with 100 ml each of saturated sodium bicarbonate solution
  7. dry with materialdried over sodium sulfate
  8. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-19a090a5a38749ddb70f39e100c2a409
출처 데이터셋
uspto-grants-1984_01
특허 번호
US04426325

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