1-(4-Chlorobenzyl)-7-cyclohexyl-1,7-diazaspiro[4.4]nonane-3,6-dione → 1-(4-Chlorobenzyl)-7-cyclohexyl-3-hydroxy-3-methyl-1,7-diazaspiro[4.4]nonan-6-one

HRID 1672395

反応式

HRID 1672395 の反応式
[CH3:1]C(=C)C[Mg]Cl.[Cl:7][C:8]1[CH:31]=[CH:30][C:11]([CH2:12][N:13]2[C:17]3([CH2:21][CH2:20][N:19]([CH:22]4[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]4)[C:18]3=[O:28])[CH2:16][C:15](=[O:29])[CH2:14]2)=[CH:10][CH:9]=1>C1COCC1>[Cl:7][C:8]1[CH:9]=[CH:10][C:11]([CH2:12][N:13]2[C:17]3([CH2:21][CH2:20][N:19]([CH:22]4[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]4)[C:18]3=[O:28])[CH2:16][C:15]([OH:29])([CH3:1])[CH2:14]2)=[CH:30][CH:31]=1

参加物

4

反応物 2

HCID 673556101-(4-Chlorobenzyl)-7-cyclohexyl-1,7-diazaspiro[4.4]nonane-3,6-dioneHCID 178448200HCID 178448200、化合物

生成物 1

HCID 673550741-(4-Chlorobenzyl)-7-cyclohexyl-3-hydroxy-3-methyl-1,7-diazaspiro[4.4]nonan-6-one

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
50 °C

実験手順

2-Methylallylmagnesium chloride in THF (3.0 M, 0.074 mL) was added to a solution of 1-(4-chlorobenzyl)-7-cyclohexyl-1,7-diazaspiro[4.4]nonane-3,6-dione (0.040 g, 0.00011 mol) in THF (1.0 mL, 0.012 mol) and the resulting mixture was stirred at 50° C. for 1 h. The reaction mixture was then allowed to cool to RT and was then quenched by the addition of saturated NH4Cl. The crude reaction mixture was purified by prep. HPLC to afford the desired product. LC/MS: 377.2 (M+1H)+.

後処理

  1. temperatureto cool to RT
  2. customwas then quenched by the addition of saturated NH4Cl
  3. customThe crude reaction mixture
  4. customwas purified by prep

出典と根拠

ORDレコード
ord-80b753a146c34d1dbd5a5a21ce81fd5c
出典データセット
uspto-grants-2011_08
特許番号
US07998959B2

関連ノート

読み込み中…