4-benzyl-N-methoxy-N-methylmorpholine-2-carboxamide → 1-(4-Benzyl-morpholin-2 yl)-pentan-1-one

HRID 30324ノート

反応式

HRID 30324 の反応式
CON(C)[C:4]([CH:6]1[O:11][CH2:10][CH2:9][N:8]([CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:7]1)=[O:5].[CH2:20]([Mg]Br)[CH2:21][CH2:22][CH3:23]>O1CCCC1>[CH2:12]([N:8]1[CH2:9][CH2:10][O:11][CH:6]([C:4](=[O:5])[CH2:20][CH2:21][CH2:22][CH3:23])[CH2:7]1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

参加物

4

反応物 2

HCID 597893084-benzyl-N-methoxy-N-methylmorpholine-2-carboxamideHCID 178418682HCID 178418682、化合物2 回

生成物 1

HCID 588548901-(4-Benzyl-morpholin-2 yl)-pentan-1-one収率 96%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Compound 82 is prepared from 2 (0.87 g, 3.28 mmol) in anhydrous tetrahydrofuran (30 mL) and commercially available (Aldrich) n-butyl magnesium bromide (2M solution in THF, 5 mmol, 2.5 mL, 1.5 eq) following General Procedure 1. After stirring for 1 hour further n-butyl magnesium bromide (2M solution in THF, 1.6 mmol, 0.8 mL) is added and stirring continued for 30 minutes. The reaction is quenched by addition of ammonium chloride solution (30 mL) followed by EtOAc. The organic phases are combined, dried over magnesium sulphate and the solvent is removed in vacuo to give 82 (0.82 g, 96%). MW 261.37; C16H23NO2; LCMS (6 minute method): m/z 262.4 [M+H]+, RT 2.34 mm.

後処理

  1. additionis added
  2. customThe reaction is quenched by addition of ammonium chloride solution (30 mL)
  3. dry with materialdried over magnesium sulphate
  4. customthe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-7ed7a8891b1a4448a61d2d6a4bb7ad15
出典データセット
uspto-grants-2008_09
特許番号
US07423037B2

反応ノート

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