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Dimethylformamide → HCID 18979151、化合物

HRID 2393188
ノート
印刷プレビュー

反応式

HRID 2393188 の反応式
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:18]2[C:27]([CH3:28])=[CH:26][C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[C:19]=2[O:29][CH3:30])[CH2:9][CH2:10][CH2:11][CH2:12][C:13]([O:15]CC)=[O:14])=[CH:4][CH:3]=1.[C:31](=O)([O-])[O-].[K+].[K+].IC.CN(C=O)C>O>[CH3:31][O:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([C:18]2[C:27]([CH3:28])=[CH:26][C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[C:19]=2[O:29][CH3:30])[CH2:9][CH2:10][CH2:11][CH2:12][C:13]([OH:15])=[O:14])=[CH:6][CH:7]=1
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 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 18979232HCID 18979232、化合物

生成物 1

HCID 18979151HCID 18979151、化合物収率 86.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Ethyl 6-(4-hydroxyphenyl)-6-(l-methoxy-3-methylnaphth-2-yl)hexanoate (30 g) was stirred with potassium carbonate (90 g), iodomethane (45 ml), and DMF (150 ml) overnight at ambient temperature. The reaction mixture was poured into cooled water and extracted with IPE. The organic layer was washed with water, dried, and evaporated. The residue was dissolved in ethanol (250 ml) and refluxed with 2.5N sodium hydroxide (250 ml) for 5 hours. Ethanol was removed and the residue was acidified with conc.HCl and extracted with ethyl acetate. The organic layer was washed with water, dried, and evaporated to give the titled compound (25 g) as crude oil.

後処理

  1. additionThe reaction mixture was poured
  2. extractionextracted with IPE
  3. washThe organic layer was washed with water
  4. customdried
  5. customevaporated
  6. dissolutionThe residue was dissolved in ethanol (250 ml)
  7. temperaturerefluxed with 2.5N sodium hydroxide (250 ml) for 5 hours
  8. customEthanol was removed
  9. extractionHCl and extracted with ethyl acetate
  10. washThe organic layer was washed with water
  11. customdried
  12. customevaporated

出典と根拠

ORDレコード
ord-759de72dc7434c6f9e0c902b0394e3f7
出典データセット
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05804601

反応ノート

読み込み中…

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