Diisopropylethylamine → HCID 69416705、化合物

HRID 915200ノート

反応式

HRID 915200 の反応式
[CH3:1][O:2][C:3](=[O:11])[CH:4]([NH2:10])[CH2:5][C:6]([CH3:9])([CH3:8])[CH3:7].CCN(C(C)C)C(C)C.[N:21]1([C:27](Cl)=[O:28])[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1>ClCCl>[CH3:1][O:2][C:3](=[O:11])[CH:4]([NH:10][C:27]([N:21]1[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1)=[O:28])[CH2:5][C:6]([CH3:7])([CH3:8])[CH3:9]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 848104-Morpholinecarbonyl chlorideHCID 23000049Methyl 2-amino-4,4-dimethylpentanoate

生成物 1

HCID 69416705HCID 69416705、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-Amino-4,4-dimethyl-pentanoic acid methyl ester (5.35 g, 27.4 mmol) was dissolved in 100 mL of dichloromethane. Hunig's base (7.07 g, 54.7 mmol) and 4-morpholinecarbonyl chloride (4.08 g, 27.4 mmol) were added and the reaction was stirred at ambient temperature 16 h. The reaction mixture was concentrated in vacuo and taken up in 150 mL EtOAc. A white precipitate formed and was filtered and washed with EtOAc. EtOAc solutions were combined and washed with 3×50 mL 1 N HCl (aq), 3×50 mL saturated NaHCO3 (aq), and 1×50 mL brine. The organic layer was dried over Na2SO4, decanted, and concentrated to a white solid (6.33 g). MS, m/z 273=M+1.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customA white precipitate formed
  3. filtrationwas filtered
  4. washwashed with EtOAc
  5. washwashed with 3×50 mL 1 N HCl (aq), 3×50 mL saturated NaHCO3 (aq), and 1×50 mL brine
  6. dry with materialThe organic layer was dried over Na2SO4
  7. customdecanted
  8. concentrationconcentrated to a white solid (6.33 g)

出典と根拠

ORDレコード
ord-bdd5b6734d0f48849356d81721dc3284
出典データセット
uspto-grants-2007_09
特許番号
US07265132B2

反応ノート

読み込み中…