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3-Ethoxy-4-methoxybenzaldehyde → 3-(3-Ethoxy-4-methoxy-benzylamino)-propionic acid ethyl ester

HRID 275893
ノート
印刷プレビュー

反応式

HRID 275893 の反応式
Cl.[CH2:2]([O:4][C:5](=[O:9])[CH2:6][CH2:7][NH2:8])[CH3:3].[CH2:10]([O:12][C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][C:20]=1[O:21][CH3:22])[CH:16]=O)[CH3:11].C([BH3-])#N.[Na+]>C(O)C>[CH2:2]([O:4][C:5](=[O:9])[CH2:6][CH2:7][NH:8][CH2:16][C:15]1[CH:18]=[CH:19][C:20]([O:21][CH3:22])=[C:13]([O:12][CH2:10][CH3:11])[CH:14]=1)[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 2447283-Ethoxy-4-methoxybenzaldehydeHCID 458475beta-Alanine, ethyl ester, hydrochlorideHCID 5003444Sodium cyanoborohydride2 回

生成物 1

HCID 538585443-(3-Ethoxy-4-methoxy-benzylamino)-propionic acid ethyl ester収率 39.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of β-alanine ethyl ester hydrochloride (1.6 g), 3-ethoxy-4-methoxybenzaldehyde (1.8 g), sodium cyanoborohydride (0.42 g) and powdered 3Å molecular seives (2.5 g) in ethanol (25 ml) was stirred at ambient temperature for 24 hours. A further aliquot of sodium cyanoborohydride (0.42 g) was added and stirring was continued for a further 24 hours. The reaction mixture was filtered and the filtrate was evaporated. The residue was treated with ethyl acetate (100 ml) and the solution was washed with 10% aqueous potassium carbonate (50 ml), then twice with water (25 ml), then with brine (25 ml), then dried over magnesium sulphate and then evaporated. The residual oil was subjected to flash chromatography on silica eluting with a mixture of dichloromethane and methanol (95:5, v/v) to give the title compound as a colourless oil (1.1 g).

後処理

  1. stirringstirring
  2. waitwas continued for a further 24 hours
  3. filtrationThe reaction mixture was filtered
  4. customthe filtrate was evaporated
  5. additionThe residue was treated with ethyl acetate (100 ml)
  6. washthe solution was washed with 10% aqueous potassium carbonate (50 ml)
  7. dry with materialtwice with water (25 ml), then with brine (25 ml), then dried over magnesium sulphate
  8. customevaporated
  9. additionThe residual oil was subjected to flash chromatography on silica eluting with a mixture of dichloromethane and methanol (95:5

出典と根拠

ORDレコード
ord-63a853df8ade4b968ea2376812013b75
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06352977B1

反応ノート

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