Ethyl formate → 5-(N-formylamino)-valeric acid ethyl ester

HRID 414737ノート

反応式

HRID 414737 の反応式
C(N(CC)CC)C.Cl.[CH2:9]([O:11][C:12](=[O:18])[CH2:13][CH2:14][CH2:15][CH2:16][NH2:17])[CH3:10].[CH2:19]([O:21]C=O)C>>[CH2:9]([O:11][C:12](=[O:18])[CH2:13][CH2:14][CH2:15][CH2:16][NH:17][CH:19]=[O:21])[CH3:10]

参加物

4

反応物 3

HCID 8025Ethyl formateHCID 8471TriethylamineHCID 16094861Ethyl 5-aminopentanoate hydrochloride

生成物 1

HCID 542728725-(N-formylamino)-valeric acid ethyl ester

実験手順

1.4 ml of triethylamine are added to 1.8 g of 5-aminovaleric acid ethyl ester hydrochloride in 40 ml of formic acid ethyl ester and the whole is then heated under reflux for 2 hours. The precipitate is filtered off, washed with a small quantity of formic acid ethyl ester and concentrated by evaporation under reduced pressure in a rotary evaporator. The residue is partitioned between methylene chloride and sodium bicarbonate solution, and the organic phase is then washed with brine, dried and concentrated by evaporation. The title compound is obtained in the form of an oil.

後処理

  1. temperaturethe whole is then heated
  2. temperatureunder reflux for 2 hours
  3. filtrationThe precipitate is filtered off
  4. washwashed with a small quantity of formic acid ethyl ester
  5. concentrationconcentrated by evaporation under reduced pressure in a rotary evaporator
  6. customThe residue is partitioned between methylene chloride and sodium bicarbonate solution
  7. washthe organic phase is then washed with brine
  8. customdried
  9. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-1ec757bc98004f3490119112f063295b
出典データセット
uspto-grants-1988_12
特許番号
US04794109

反応ノート

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