4-Methylmorpholine → Ethyl N-(1-((benzyloxy)carbonyl)-L-prolyl)-L-leucinate

HRID 1733664

반응식

HRID 1733664 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:18][CH2:17][CH2:16][C@H:12]1[C:13]([OH:15])=O)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH2:20]([O:22][C:23](=[O:30])[C@H:24]([CH2:26][CH:27]([CH3:29])[CH3:28])[NH2:25])[CH3:21].CN1CCOCC1.O=C1C2C=CC=CC=2N=NN1OS(C)(=O)=O>C(Cl)(Cl)Cl.C(OCC)(=O)C.O>[CH2:20]([O:22][C:23](=[O:30])[C@H:24]([CH2:26][CH:27]([CH3:29])[CH3:28])[NH:25][C:13](=[O:15])[C@@H:12]1[CH2:16][CH2:17][CH2:18][N:11]1[C:9]([O:8][CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)=[O:10])[CH3:21]

참가 물질

8

반응물 4

HCID 79724-MethylmorpholineHCID 101987Benzyloxycarbonyl-L-prolineHCID 11658447L-Leucine, ethyl ester, hydrochloride (1:1)HCID 218962814-Oxo-3,4-dihydro-3-methanesulfonyloxy-1,2,3-benzotriazine

생성물 1

HCID 6453075Ethyl N-(1-((benzyloxy)carbonyl)-L-prolyl)-L-leucinate수율 66.4%

시약·촉매·용매 3

HCID 962Water용매HCID 6212Chloroform용매HCID 8857Ethyl Acetate용매

실험 절차

N-Benzyloxycarbonyl-L-proline (1.25 g), L-leucine ethyl ester hydrochloride (1.00 g) and N-methylmorpholine (1.10 ml) are dissolved in chloroform (10 ml) and thereto is added 4-oxo-3,4-dihydro-3-methanesulfonyloxy-1,2,3-benzotriazine (1.20 g). After allowing to stand overnight, to the mixture are added water and ethyl acetate. The ethyl acetate layer is washed and dried, and then the solvent is distilled off to give N-(N-benzyloxycarbonyl-L-prolyl)-L-leucine ethyl ester (1.3 g), melting point: 65°-67° C.

후처리

  1. washThe ethyl acetate layer is washed
  2. customdried
  3. distillationthe solvent is distilled off

출처 및 근거

ORD 기록
ord-89cf0924f3e74005978288a0de1fd424
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04242507

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