Tridecanal → Methyl 3-tridecylaminopropionate

HRID 1872802ノート

反応式

HRID 1872802 の反応式
[CH:1](=O)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].Cl.[NH2:16][CH2:17][CH2:18][C:19]([O:21][CH3:22])=[O:20].C([O-])(=O)C.[Na+].C([BH3-])#N.[Na+]>CO>[CH2:1]([NH:16][CH2:17][CH2:18][C:19]([O:21][CH3:22])=[O:20])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

参加物

6

反応物 4

HCID 25311TridecanalHCID 517045Sodium AcetateHCID 2734767Methyl 3-aminopropanoate hydrochlorideHCID 5003444Sodium cyanoborohydride

生成物 1

HCID 18687169Methyl 3-tridecylaminopropionate収率 54.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To an ice-cooled solution of tridecanal (1.0 g), methyl 3-aminopropionate hydrochloride (704 mg), and sodium acetate (414 mg) in methanol (20 ml) was added sodium cyanoborohydride (317 mg). After stirring for 45 minutes, the mixture was quenched with water (20 ml), concentrated, and extracted with ethyl acetate (40 ml). The organic phase was washed with brine, dried, and concentrated under reduced pressure. The residue was purified on silica gel, eluting with 5% methanol in chloroform to give methyl 3-tridecylaminopropionate (0.78 g).

後処理

  1. customthe mixture was quenched with water (20 ml)
  2. concentrationconcentrated
  3. extractionextracted with ethyl acetate (40 ml)
  4. washThe organic phase was washed with brine
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified on silica gel
  8. washeluting with 5% methanol in chloroform

出典と根拠

ORDレコード
ord-e5abfdbc0abf41a093719ba20cb5e680
出典データセット
uspto-grants-2000_08
特許番号
US06110933

反応ノート

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