Ammonium Hydroxide → Oxane-4-carboxamide

HRID 9469

反応式

HRID 9469 の反応式
[OH-].[NH4+:2].[O:3]1[CH2:8][CH2:7][CH:6]([C:9]([O:11]C)=O)[CH2:5][CH2:4]1>CO>[O:3]1[CH2:8][CH2:7][CH:6]([C:9]([NH2:2])=[O:11])[CH2:5][CH2:4]1

参加物

4

実験手順

Ammonium hydroxide (1 L) was added to a solution of methyl tetrahydro-2H-pyran-4-carboxylate (20 mL, 150 mmol) in methanol (500 mL), and the reaction was stirred overnight at ambient temperature. Additional ammonium hydroxide (500 mL) was added, and the reaction was stirred for four additional days. The methanol was removed under reduced pressure. Solid sodium chloride was added to the aqueous layer, which was extracted with chloroform (3×150 mL). The combined extracts were dried over sodium sulfate, filtered, and concentrated under reduced pressure to provide 11.4 g of tetrahydropyran-4-carboxamide as a white solid.

後処理

  1. stirringthe reaction was stirred for four additional days
  2. customThe methanol was removed under reduced pressure
  3. additionSolid sodium chloride was added to the aqueous layer, which
  4. extractionwas extracted with chloroform (3×150 mL)
  5. dry with materialThe combined extracts were dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-5574c035cb5d4caf8df4dacdca15baab
出典データセット
uspto-grants-2006_08
特許番号
US07091214B2

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