Benzaldehyde → (Z)-1-Acetyl-3-benzylidenepiperazine-2,5-dione

HRID 442652노트

반응식

HRID 442652 반응식
C([N:4]1[CH2:9][C:8](=[O:10])[N:7]([C:11](=[O:13])[CH3:12])[CH2:6][C:5]1=[O:14])(=O)C.C(N(CC)CC)C.[CH:22](=O)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.CCOC(C)=O>CN(C=O)C>[C:11]([N:7]1[CH2:6][C:5](=[O:14])[NH:4]/[C:9](=[CH:22]\[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)/[C:8]1=[O:10])(=[O:13])[CH3:12]

참가 물질

6

반응물 4

HCID 240BenzaldehydeHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 5403711,4-Diacetyl-2,5-piperazinedione

생성물 1

HCID 5915153(Z)-1-Acetyl-3-benzylidenepiperazine-2,5-dione

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1,4-Diacetyl-2,5-piperazinedione (25.0 g, 126 mmol), which is compound (8) mentioned in Reference Example 3, was heated at 120°-130° C. in DMF (200 ml) with triethylamine (17.6 ml, 126 mmol) and benzaldehyde (13.0 ml, 126 mmol). After 4 h the mixture was cooled to room temperature and poured into EtOAc (1000 ml), and washed three times with brine. Any solid formed at this stage was filtered off.

후처리

  1. washwashed three times with brine
  2. customAny solid formed at this stage
  3. filtrationwas filtered off

출처 및 근거

ORD 기록
ord-62547bda284249ac8cb248340172cbed
출처 데이터셋
uspto-grants-1999_04
특허 번호
US05891877

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