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

HRID 442652ノート

反応式

HRID 442652 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-62547bda284249ac8cb248340172cbed
出典データセット
uspto-grants-1999_04
特許番号
US05891877

反応ノート

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