Maleic Acid → HCID 70403916、化合物

HRID 4368ノート

反応式

HRID 4368 の反応式
[C:1]([O:5][C:6](=[O:17])[C@@H:7]1[CH2:11][CH2:10][CH2:9][N:8]1[C:12](=[O:16])[C@H:13]([CH3:15])[NH2:14])([CH3:4])([CH3:3])[CH3:2].[CH2:18]([O:20][C:21](=[O:32])/[CH:22]=[CH:23]/[C:24](=[O:31])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[CH3:19].[C:33]([OH:40])(=[O:39])/[CH:34]=[CH:35]\[C:36]([OH:38])=[O:37]>C1C=CC=CC=1>[C:33]([OH:40])(=[O:39])/[CH:34]=[CH:35]\[C:36]([OH:38])=[O:37].[C:1]([O:5][C:6](=[O:17])[C@@H:7]1[CH2:11][CH2:10][CH2:9][N:8]1[C:12](=[O:16])[C@H:13]([CH3:15])[NH:14][C@H:22]([C:21]([O:20][CH2:18][CH3:19])=[O:32])[CH2:23][C:24]([C:25]1[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1)=[O:31])([CH3:2])([CH3:4])[CH3:3]

参加物

5

反応物 3

HCID 444266Maleic AcidHCID 5369605Ethyl (2E)-4-oxo-4-phenyl-2-butenoateHCID 12939800tert-Butyl L-alanyl-L-prolinate

生成物 1

HCID 70403916HCID 70403916、化合物収率 60%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

4.84 g (20 mmoles) of (S)-alanyl-(S)-proline-t-butylester are dissolved in 40 ml of dry benzene and 4.08 g (20 mmoles) of E-ethyl-3-benzoyl-acrylate are added at room temperature under stirring. After one hour stirring at room temperature the solvent is evaporated off under reduced pressure, the residue is dissolved in 20 ml of ethyl acetate and 2.32 g (20 mmoles) of maleinic acid are added. The precipitated crystals are filtered off after one hour standing and washed with 20 ml of ethyl acetate. 6.7 g (60%) of product are obtained with a melting point of 109°-110° C.

後処理

  1. stirringAfter one hour stirring at room temperature the solvent
  2. customis evaporated off under reduced pressure
  3. dissolutionthe residue is dissolved in 20 ml of ethyl acetate
  4. filtrationThe precipitated crystals are filtered off after one hour standing
  5. washwashed with 20 ml of ethyl acetate

出典と根拠

ORDレコード
ord-f01be8f761ca4562ae3496ae6ef3ae07
出典データセット
uspto-grants-1988_02
特許番号
US04725617

反応ノート

読み込み中…