反応 #1227

ord-d9af6adb5c534d1a86a82222f63dd4ec

反応方程式

O
water
[H-].[Na+]
sodium hydride
COC(=O)c1ccc(-c2ccc3cc4c(cc3c2)C(C)(C)CCC4(C)C)cc1O
methyl 2-hydroxy-4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-anthryl)benzoate
CI
iodomethane
COC(=O)c1ccc(-c2ccc3cc4c(cc3c2)C(C)(C)CCC4(C)C)cc1OC
methyl 2-methoxy-4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-anthryl)benzoate

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGthe mixture was stirred at room temperature for two hours
  2. 2
    抽出extracted with ethyl ether
  3. 3
    その他the organic phase decanted
  4. 4
    乾燥dried over magnesium sulfate
  5. 5
    その他evaporated
  6. 6
    その他1.6 g (96%) of the expected compound was recovered in the form of a colorless oil

実験手順

130 mg (4.2 mmol) of sodium hydride (80% in oil) and 20 ml of DMF were introduced into a three-necked flask, a solution of 1.6 g (4.2 mmol) of methyl 2-hydroxy-4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-anthryl)benzoate in 50 ml of DMF was added dropwise and the mixture was stirred until gaseous emission ceased. 340 μl (5.5 mmol) of iodomethane were then added and the mixture was stirred at room temperature for two hours. The reaction medium was poured into water, extracted with ethyl ether, the organic phase decanted, dried over magnesium sulfate and evaporated. 1.6 g (96%) of the expected compound was recovered in the form of a colorless oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05723499uspto-grants-1998_03