Water → 1-Acetyl-3-(4-tert-butyldiphenylsilyloxymethyl-3-methylphenyl)methylene-2,5-piperazinedione

HRID 584214ノート

反応式

HRID 584214 の反応式
[Si:1]([O:18][CH2:19][C:20]1[CH:27]=[CH:26][C:23]([CH:24]=O)=[CH:22][C:21]=1[CH3:28])([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:29]([N:32]1[CH2:37][C:36](=[O:38])[N:35](C(=O)C)[CH2:34][C:33]1=[O:42])(=[O:31])[CH3:30].CC(C)([O-])C.[K+].O>CN(C)C=O.C(O)(C)(C)C>[C:29]([N:32]1[CH2:37][C:36](=[O:38])[NH:35][C:34](=[CH:24][C:23]2[CH:26]=[CH:27][C:20]([CH2:19][O:18][Si:1]([C:14]([CH3:15])([CH3:16])[CH3:17])([C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)=[C:21]([CH3:28])[CH:22]=2)[C:33]1=[O:42])(=[O:31])[CH3:30]

参加物

7

反応物 4

HCID 962WaterHCID 5403711,4-Diacetyl-2,5-piperazinedioneHCID 223429234-(Tert-butyldiphenylsilyloxymethyl)-3-methylbenzaldehydeHCID 23665647Potassium tert-butoxide

生成物 1

HCID 696776911-Acetyl-3-(4-tert-butyldiphenylsilyloxymethyl-3-methylphenyl)methylene-2,5-piperazinedione収率 71.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6386tert-Butanol溶媒

実験手順

To a stirred mixture of 4-(tert-butyldiphenylsilyloxymethyl)-3-methylbenzaldehyde (1.94 g) and 1,4-diacetyl-2,5-piperazinedione (991 mg) in a mixture of N,N-dimethylformamide (10 ml) and tert-butanol (10 ml) was added potassium tert-butoxide (561 mg) at 5° C. The mixture was stirred for 1 hour at room temperature and then poured into water (300 ml), and stirring was continued for 18 hours at room temperature. The resulting precipitates were collected by filtration and washed with water and isopropyl ether, and dried under reduced pressure to give 1-acetyl-3-(4-tert-butyldiphenylsilyloxymethyl-3-methylphenyl)methylene-2,5-piperazinedione (1.88 g) as a powder.

後処理

  1. stirringstirring
  2. waitwas continued for 18 hours at room temperature
  3. customThe resulting precipitates
  4. filtrationwere collected by filtration
  5. washwashed with water and isopropyl ether
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-de72eff2dc114209b7ca7de62477dd76
出典データセット
uspto-grants-2005_08
特許番号
US06924278B2

反応ノート

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