Potassium Carbonate → 6-Ethynyl-2,2-dimethylchroman-4-one

HRID 619648ノート

反応式

HRID 619648 の反応式
[CH3:1][C:2]1([CH3:19])[CH2:11][C:10](=[O:12])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:13]#[C:14][Si](C)(C)C)[CH:8]=2)[O:3]1.C([O-])([O-])=O.[K+].[K+]>CO.CCOC(C)=O>[CH3:1][C:2]1([CH3:19])[CH2:11][C:10](=[O:12])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:13]#[CH:14])[CH:8]=2)[O:3]1

参加物

5

反応物 2

HCID 11430Potassium CarbonateHCID 218466592,2-Dimethyl-6-trimethylsilanylethynyl-chroman-4-one2 回

生成物 1

HCID 218466816-Ethynyl-2,2-dimethylchroman-4-one収率 91%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2,2-dimethyl-6-trimethylsilanylethynyl-chroman-4-one (Compound 261, 4.05 g, 14.87 mmol) in 60.0 mL of MeOH was added K2CO3 (410.9 mg, 2.97 mmol) The resulting mixture was stirred at room temperature for 24 hours, diluted with EtOAc (100 mL) and washed with H2O and saturated aqueous NaCl, and dried over Na2SO4. Concentration of this solution under reduced pressure afforded 2.71 g (91%) of the product as a tan solid. 1H NMR (300 MHz, CDCl3) δ: 8.01 (1H, d, J=2.2 Hz), 7.56 (1H, dd, J=2.2, 8.6 Hz), 6.90 (1H, d, J=8.6 Hz), 3.02 (1H, s), 2.74 (2H, s), 1.47 (6H, s).

後処理

  1. washwashed with H2O and saturated aqueous NaCl
  2. dry with materialdried over Na2SO4

出典と根拠

ORDレコード
ord-2907a7adb8414ae3938bbffaabc33c4f
出典データセット
uspto-grants-1999_09
特許番号
US05958954

反応ノート

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