Triethylamine → 2-Methoxy-8-methylcarbamoyl-2,8-diazaspiro[4,5]decane-1,3-dione

HRID 1381942ノート

反応式

HRID 1381942 の反応式
Cl.[CH3:2][O:3][N:4]1[C:8](=[O:9])[CH2:7][C:6]2([CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[C:5]1=[O:15].C(N(CC)CC)C.[CH3:23][N:24]=[C:25]=[O:26]>O>[CH3:2][O:3][N:4]1[C:8](=[O:9])[CH2:7][C:6]2([CH2:14][CH2:13][N:12]([C:25](=[O:26])[NH:24][CH3:23])[CH2:11][CH2:10]2)[C:5]1=[O:15]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 12228Methyl IsocyanateHCID 30882852,8-Diazaspiro(4,5)decane-1,3-dione, 2-methoxy-, monohydrochloride

生成物 1

HCID 212754282-Methoxy-8-methylcarbamoyl-2,8-diazaspiro[4,5]decane-1,3-dione

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 2-methoxy-2,8-diazaspiro[4,5]decane-1,3-dione hydrochloride (1.5 g) in water (20 ml) was added triethylamine (1 ml), followed by methyl isocyanate (1 ml), and this was followed by stirring at room temperature for 30 minutes. The water was then evaporated off under reduced pressure. The residue was directly subjected to silica gel column chromatography (eluent; chloroform-acetone-methanol=10:3:2 (v/v)), and the solvent for the solution containing the desired product was evaporated off under reduced pressure to obtain 1.4 g of a colorless oily compound.

後処理

  1. customThe water was then evaporated off under reduced pressure
  2. additionthe solvent for the solution containing the desired product
  3. customwas evaporated off under reduced pressure

出典と根拠

ORDレコード
ord-eafad1bcea084cac804c664897443a18
出典データセット
uspto-grants-1989_02
特許番号
US04804665

反応ノート

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