Water → HCID 21190099、化合物

HRID 619509ノート

反応式

HRID 619509 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 21190099HCID 21190099、化合物収率 31.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3e32a66a57b7461990ce493b108316aa
出典データセット
uspto-grants-1999_09
特許番号
US05958942

反応ノート

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