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

HRID 1733664

反応式

HRID 1733664 の反応式
[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]

参加物

8

反応物 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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6212Chloroform溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-89cf0924f3e74005978288a0de1fd424
出典データセット
uspto-grants-1980_12
特許番号
US04242507

関連ノート

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