Maleic Acid → HCID 70403916, 화합물

HRID 4368노트

반응식

HRID 4368 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 70403916HCID 70403916, 화합물수율 60%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f01be8f761ca4562ae3496ae6ef3ae07
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725617

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