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[4-(Methoxycarbonyl)benzyl](triphenyl)phosphonium bromide → HCID 14726493、化合物

HRID 1614094
ノート
印刷プレビュー

反応式

HRID 1614094 の反応式
C([O-:5])(C)(C)C.[K+].[Br-].[C:8]([C:12]1[CH:37]=[CH:36][C:15]([CH2:16][P+](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=[CH:14][CH:13]=1)([O:10][CH3:11])=[O:9].[CH3:38][C:39]1([CH3:54])[CH2:48][CH2:47][C:46]([CH3:50])([CH3:49])[C:45]2[CH:44]=[C:43]([C:51](Cl)=[O:52])[CH:42]=[CH:41][C:40]1=2>C1(C)C=CC=CC=1>[C:8]([C:12]1[CH:13]=[CH:14][C:15]([C:16](=[O:5])[C:51]([C:43]2[CH:42]=[CH:41][C:40]3[C:39]([CH3:54])([CH3:38])[CH2:48][CH2:47][C:46]([CH3:50])([CH3:49])[C:45]=3[CH:44]=2)=[O:52])=[CH:36][CH:37]=1)([O:10][CH3:11])=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 2764257[4-(Methoxycarbonyl)benzyl](triphenyl)phosphonium bromideHCID 27954665,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalene-2-carbonyl chlorideHCID 23665647Potassium tert-butoxide

生成物 1

HCID 14726493HCID 14726493、化合物収率 12%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

7.9 g (33 mmol) of potassium tert-butanolate were added a little at a time to a suspension of 34.5 g (66 mmol) of 4-carbomethoxybenzyltriphenylphosphonium bromide were added in 200 ml of dry toluene at room temperature. The mixture was stirred for 10 min and then heated to reflux, and 7.5 g (33 mmol) of 5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthalene-2-carbonyl chloride were added dropwise. After the solution had become colorless again it was allowed to cool and solids were filtered off. The filtrate was concentrated, and the remaining oil was recrystallized from methanol (11.2 g of the ylide intermediate of melting point 101°-203° C.). 3.2 g of the ylide and 3.1 g of sodium periodate were refluxed in a mixture of 40 ml of ethanol and 10 ml of water for 1 h. Saturated brine was added to the cooled reaction mixture, which was then extracted with methylene chloride. The organic phase was dried over magnesium sulfate and concentrated. The residue was triturated in n-heptane, the solids were filtered off, and the filtrate was concentrated. Recrystallization from ethanol yielded 1.5 g of the title compound of melting point 93°-96° C.

後処理

  1. temperatureheated
  2. temperatureto reflux
  3. temperatureto cool
  4. filtrationsolids were filtered off
  5. concentrationThe filtrate was concentrated
  6. customthe remaining oil was recrystallized from methanol (11.2 g of the ylide intermediate of melting point 101°-203° C.)
  7. temperature3.2 g of the ylide and 3.1 g of sodium periodate were refluxed in a mixture of 40 ml of ethanol and 10 ml of water for 1 h
  8. additionSaturated brine was added to the cooled reaction mixture, which
  9. extractionwas then extracted with methylene chloride
  10. dry with materialThe organic phase was dried over magnesium sulfate
  11. concentrationconcentrated
  12. customThe residue was triturated in n-heptane
  13. filtrationthe solids were filtered off
  14. concentrationthe filtrate was concentrated
  15. customRecrystallization from ethanol

出典と根拠

ORDレコード
ord-4ce53c562a9a4a70bdb057e86577cf6b
出典データセット
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05194664

反応ノート

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