Water → HCID 21190099, 화합물

HRID 619509노트

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HRID 619509 반응식
[CH3:1][C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][CH:10]=[C:9]3[N:5]2[C:6]=1[C:7](=[O:13])[NH:8]3.[H-].[Na+].Br[CH2:17][CH2:18][CH2:19][N:20]1[C:24](=[O:25])[C:23]2=[CH:26][CH:27]=[CH:28][CH:29]=[C:22]2[C:21]1=[O:30].O>CN(C=O)C>[CH3:1][C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][CH:10]=[C:9]3[N:5]2[C:6]=1[C:7](=[O:13])[N:8]3[CH2:17][CH2:18][CH2:19][N:20]1[C:24](=[O:25])[C:23]2=[CH:26][CH:27]=[CH:28][CH:29]=[C:22]2[C:21]1=[O:30]

참가 물질

6

반응물 4

HCID 962WaterHCID 21611N-3-BromopropylphthalimideHCID 24758Sodium hydrideHCID 1358102941,2-Dihydro-3-methyl-1,4,7b-triazacyclopent[cd)inden-2-one

생성물 1

HCID 21190099HCID 21190099, 화합물수율 31.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a suspension of 8.66 g (50 mmol) of 1,2-dihydro-3-methyl-1,4,7b-triazacyclopent[cd]inden-2-one in 100 ml of DMF was added, while stirring under ice-cooling, 2.20 g (55 mmol) of 60% sodium hydride (dispersion in oil). The mixture was stirred for 20 minutes at the same temperature. To the reaction mixture was added 13.14 g (50 mmol) of N-(3-bromopropyl)phthalimide. The mixture was stirred for 7 hours at 100° C. After cooling, the reaction mixture was poured into water, which was subjected to extraction with chloroform. The extract was dried over anhydrous magnesium sulfate, and, the solvent was then distilled off. The residue was crystallized from methylene chloride--ethanol to give 5.72 g of the desired compound (31.7%, pale brown solid substance).

후처리

  1. additionwas added
  2. temperaturecooling
  3. stirringThe mixture was stirred for 20 minutes at the same temperature
  4. stirringThe mixture was stirred for 7 hours at 100° C
  5. temperatureAfter cooling
  6. extractionwas subjected to extraction with chloroform
  7. dry with materialThe extract was dried over anhydrous magnesium sulfate
  8. distillationthe solvent was then distilled off
  9. customThe residue was crystallized from methylene chloride

출처 및 근거

ORD 기록
ord-3e32a66a57b7461990ce493b108316aa
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05958942

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