Hydrochloric Acid → 2-methyl-2H-pyran-3,5(4H,6H)-dione

HRID 478304ノート

反応式

HRID 478304 の反応式
CC(C)([O-])C.[K+].[CH3:7][CH:8]([O:12][CH2:13][C:14]([O:16]C)=O)[C:9](=[O:11])[CH3:10].Cl>C(O)(C)(C)C.CCOCC>[CH3:7][CH:8]1[C:9](=[O:11])[CH2:10][C:14](=[O:16])[CH2:13][O:12]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 23665647Potassium tert-butoxideHCID 71360827Methyl (1-methyl-2-oxopropoxy)acetate

生成物 1

HCID 234974742-methyl-2H-pyran-3,5(4H,6H)-dione

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 6386tert-Butanol溶媒

反応条件

温度
0 °C

実験手順

A mechanically stirred solution of potassium tert-butoxide in tert-butanol (1 M, 203 mL) under a nitrogen atmosphere was treated with anhydrous ether (125 mL), cooled to 0° C., treated with the product from Example 84B (15.5 g, 97 mmol) in ether (55 mL) over 2 minutes, stirred for 10 minutes and then treated with 2M HCl (240 mL). The layers were separated and the aqueous layer was extracted with ethyl acetate (2×, 200 mL). The combined organic layers were washed with brine, dried (MgSO4), filtered and concentrated. The residue was purified on silica gel eluting with ethyl acetate:formic acid:water:hexane (200:1:1:200) to provide the title compound.

後処理

  1. customThe layers were separated
  2. extractionthe aqueous layer was extracted with ethyl acetate (2×, 200 mL)
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified on silica gel eluting with ethyl acetate:formic acid:water:hexane (200:1:1:200)

出典と根拠

ORDレコード
ord-dfd519c5d71d45d4abf893a9c116b05b
出典データセット
uspto-grants-2003_11
特許番号
US06642222B2

反応ノート

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