Monoethyl malonate → HCID 54441812、化合物

HRID 850633ノート

反応式

HRID 850633 の反応式
[O:1]1[C:5]2=[N:6][CH:7]=[C:8]([CH:10]=O)[CH:9]=[C:4]2[CH:3]=[CH:2]1.[C:12]([O:18][CH2:19][CH3:20])(=[O:17])[CH2:13]C(O)=O.C([O-])(=O)C.[NH4+:25]>C(O)C>[CH2:19]([O:18][C:12](=[O:17])[CH2:13][CH:10]([NH2:25])[C:8]1[CH:9]=[C:4]2[CH:3]=[CH:2][O:1][C:5]2=[N:6][CH:7]=1)[CH3:20]

参加物

5

反応物 3

HCID 70615Monoethyl malonateHCID 517165Ammonium AcetateHCID 10749327furo[2,3-b]pyridine-5-carbaldehyde

生成物 1

HCID 54441812HCID 54441812、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution containing aldehyde 23-2 (1.5 g, 10 mmol), ethyl hydrogen malonate (1.6 g, 20 mmol), and ammonium acetate (3.8 g, 50 mmol) in anhydrous ethanol (125 mL) was heated at reflux for 8 h. After cooling to room temperature, the solvent was evaporated and the residue partitioned between sat. sodium bicarbonate and EtOAc, the organic layer removed, dried, and concentrated. Chromatography of the residue afforded the amino ester 23-3 as a waxy solid.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 8 h
  3. customthe solvent was evaporated
  4. customthe residue partitioned between sat. sodium bicarbonate and EtOAc
  5. customthe organic layer removed
  6. customdried
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-5040458b951c433abc46dcedbaf49d2d
出典データセット
uspto-grants-2000_01
特許番号
US06017926

反応ノート

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