1,3-Dibromopropane → HCID 20427608, 화합물

HRID 615316노트

반응식

HRID 615316 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 20427608HCID 20427608, 화합물수율 67.8%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-846fb5838c8b48beb819b2e17b18e5c6
출처 데이터셋
uspto-grants-1985_02
특허 번호
US04499089

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