反応 #7120

ord-fc1c3c23629140928ac9e042705804cc

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The reaction was concentrated to dryness in vacuo
  2. 2
    その他azeotroped with toluene (50 mL)
  3. 3
    その他The crude product, cis-2-aminocyclohexanecarboxylic acid amide, was used in the next reaction without purification

実験手順

cis-2-Aminocyclohexanecarboxylic acid methyl ester (2.20 g, 14.0 mmol) was treated with aqueous ammonium hydroxide (40 mL) in toluene (40 mL) and stirred vigorously at room temperature for 16 h. The reaction was concentrated to dryness in vacuo and azeotroped with toluene (50 mL). The crude product, cis-2-aminocyclohexanecarboxylic acid amide, was used in the next reaction without purification: 1H NMR (400 MHz, DMSO-d6) δ 7.78 (2 H, s br), 7.67 (s, 1 H), 7.25 (s, 1 H), 1.87 (m, 2 H), 1.60 (m, 4 H), 1.41 (m, 4 H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07084178B2uspto-grants-2006_08