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

HRID 2295709

反応式

HRID 2295709 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-19a090a5a38749ddb70f39e100c2a409
出典データセット
uspto-grants-1984_01
特許番号
US04426325

関連ノート

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