Monoethyl malonate → HCID 54441812、化合物

HRID 1387471ノート

反応式

HRID 1387471 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 22-2 (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 22-3 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-a75ef70b884a448a8cc31d2a617658cd
出典データセット
uspto-grants-2001_07
特許番号
US06268378B1

反応ノート

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