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Furfural → Ethyl 3-[(furan-2-ylmethylene)amino]propanoate

HRID 1511599
ノート
印刷プレビュー

反応式

HRID 1511599 の反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=O.S([O-])([O-])(=O)=O.[Mg+2].C(N(CC)CC)C.Cl.[NH2:22][CH2:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26]>C(Cl)Cl.O>[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]=[N:22][CH2:23][CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7362FurfuralHCID 8471TriethylamineHCID 24083Sulfuric acid magnesium salt (1:1)HCID 458475beta-Alanine, ethyl ester, hydrochloride

生成物 1

HCID 68410140Ethyl 3-[(furan-2-ylmethylene)amino]propanoate収率 94.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6344Dichloromethane溶媒

実験手順

2-Furaldehyde (10 g) was dissolved in 170 mL of methylene chloride, then 10 g of magnesium sulfate, 16 mL of triethylamine and 16 g of ethyl 3-aminopropionate hydrochloride were successively added thereto and the mixture was stirred overnight at room temperature. The reaction solution was poured over 100 mL of water, the mixture was subjected to extraction with methylene chloride and the solvent was evaporated therefrom in vacuo. The residue was dissolved in 100 mL of ethyl acetate, washed with water and a saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom in vacuo to give 19.2 g of the objective compound as yellow liquid.

後処理

  1. extractionthe mixture was subjected to extraction with methylene chloride
  2. customthe solvent was evaporated
  3. dissolutionThe residue was dissolved in 100 mL of ethyl acetate
  4. washwashed with water
  5. dry with materiala saturated solution of sodium chloride successively and dried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-b8e12db1887a499a9302d71a70cd273b
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217031B2

反応ノート

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