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

HRID 584214노트

반응식

HRID 584214 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6386tert-Butanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-de72eff2dc114209b7ca7de62477dd76
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06924278B2

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