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Propargyl bromide → 6-Ethyl-5-methyl-2-phenyl-3-propargyl-5,6-dihydropyrimidin-4-one

HRID 1779889
ノート
印刷プレビュー

反応式

HRID 1779889 の反応式
[CH2:1]([Li])[CH2:2][CH2:3]C.[CH2:6]([CH:8]1[NH:13][C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[N:11][C:10](=[O:20])[CH:9]1[CH3:21])[CH3:7].C(Br)C#C>O1CCCC1.C1(C)C=CC=CC=1>[CH2:6]([CH:8]1[N:13]=[C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:11]([CH2:3][C:2]#[CH:1])[C:10](=[O:20])[CH:9]1[CH3:21])[CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7842Propargyl bromideHCID 178418339ButyllithiumHCID 178437565HCID 178437565、化合物

生成物 1

HCID 190485476-Ethyl-5-methyl-2-phenyl-3-propargyl-5,6-dihydropyrimidin-4-one

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Oven dried glassware and a nitrogen purge were utilized. 3.22 mL of 1.6 Molar n-butyl lithium in hexanes (5.15 mmol) was added dropwise to a solution of 1.06 g (4.93 mmol) of 6-ethyl-5-methyl-2-phenyl-5,6-dihydropyrimidin-4-one, in 15 mL of dry tetrahydrofuran, at -50 to -60° C. The mixture was stirred for 15 minutes and then 0.8 mL (5.38 mmol) of 80 wt.% propargyl bromide in toluene was added at -65° C. The ice bath was removed after 1.5 hours and the reaction mixture was stirred for an additional 20 hours. The solvent had evaporated overnight. Ether was added and the reaction mixture was washed three times with water followed by three times with 3 Molar hydrochloric acid. The acidic aqueous washes were combined, cooled externally, and 50% sodium hydroxide was added until the pH=10, then extracted three times with ether. The ether extracts were combined, dried over magnesium sulfate, and concentrated to yield 0.68 g of crude product. The crude product was combined with crude product obtained from previous reactions and purified on a six inch plug of basic alumina by washing with 400 mL of methylene chloride. The filtrate was concentrated to yield 6-ethyl-5-methyl-2-phenyl-3-propargyl-5,6-dihydropyrimidin-4-one (Compound 1), as a yellow solid, melting 62°-65° C.

後処理

  1. customOven dried glassware
  2. customa nitrogen purge
  3. customThe ice bath was removed after 1.5 hours
  4. stirringthe reaction mixture was stirred for an additional 20 hours
  5. customThe solvent had evaporated overnight
  6. additionEther was added
  7. washthe reaction mixture was washed three times with water
  8. temperaturecooled externally
  9. addition50% sodium hydroxide was added until the pH=10
  10. extractionextracted three times with ether
  11. dry with materialdried over magnesium sulfate
  12. concentrationconcentrated
  13. customto yield 0.68 g of crude product
  14. customobtained from previous reactions
  15. custompurified on a six inch plug of basic alumina
  16. washby washing with 400 mL of methylene chloride
  17. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-7062b6c48e744b8db12b300fbbd1e4f1
出典データセット
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05629264

反応ノート

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