1,3-Dibromopropane → HCID 20427608、化合物

HRID 615316ノート

反応式

HRID 615316 の反応式
[CH2:1]([S:3][C:4]1[NH:5][C:6](=[O:23])[C:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8]=1[C:9]#[N:10])[CH3:2].[H-].[Na+].[Br:26][CH2:27][CH2:28][CH2:29]Br>O1CCOCC1>[Br:26][CH2:27][CH2:28][CH2:29][N:5]1[C:6](=[O:23])[C:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8]([C:9]#[N:10])=[C:4]1[S:3][CH2:1][CH3:2]

参加物

5

反応物 3

HCID 80011,3-DibromopropaneHCID 24758Sodium hydrideHCID 132361792-(Ethylsulfanyl)-5-oxo-4,4-diphenyl-4,5-dihydro-1H-pyrrole-3-carbonitrile

生成物 1

HCID 20427608HCID 20427608、化合物収率 67.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

One dissolves 15.0 g 2-ethylthio-5-oxo-4,4-diphenyl-2-pyrroline-3-carbonitrile in 500 ml abs. dioxan, adds 1.4 g sodium hydride (80%) in white oil) thereto and boils under reflux for one hour. One allows to cool somewhat, adds 100.0 g 1,3-dibromopropane thereto and further boils for 48 hours. Thereafter, the reaction mixture is filtered, the solvent and the excess dibromopropane are distilled off under water pump vacuum and the residue is triturated with diisopropyl ether. One obtains 14.0 g 1-(3-bromopropyl)-2-ethylthio-5-oxo-4,4-diphenyl-2-pyrroline-3-carbonitrile of mp 97° C.

後処理

  1. temperatureunder reflux for one hour
  2. temperatureto cool somewhat
  3. filtrationThereafter, the reaction mixture is filtered
  4. distillationthe solvent and the excess dibromopropane are distilled off under water pump vacuum
  5. customthe residue is triturated with diisopropyl ether

出典と根拠

ORDレコード
ord-846fb5838c8b48beb819b2e17b18e5c6
出典データセット
uspto-grants-1985_02
特許番号
US04499089

反応ノート

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