HCID 57718998、化合物 → HCID 10195632、化合物

HRID 1985123ノート

反応式

HRID 1985123 の反応式
C([O:3][C:4](=[O:37])[C:5]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][CH2:16][CH2:17][CH:18]2[CH2:22][N:21]([CH2:23][C:24]3[CH:29]=[CH:28][C:27]([C:30]([CH3:33])([CH3:32])[CH3:31])=[CH:26][CH:25]=3)[C:20](=[O:34])[N:19]2[CH3:35])=[CH:11][C:10]=1[CH3:36])([CH3:7])[CH3:6])C>CO>[C:30]([C:27]1[CH:28]=[CH:29][C:24]([CH2:23][N:21]2[CH2:22][CH:18]([CH2:17][CH2:16][CH2:15][C:12]3[CH:13]=[CH:14][C:9]([O:8][C:5]([CH3:6])([CH3:7])[C:4]([OH:37])=[O:3])=[C:10]([CH3:36])[CH:11]=3)[N:19]([CH3:35])[C:20]2=[O:34])=[CH:25][CH:26]=1)([CH3:31])([CH3:32])[CH3:33]

参加物

3

反応条件

温度
0 °C

実験手順

2-(4-{3-[1-(4-tert-Butyl-benzyl)-3-methyl-2-oxo-imidazolidin-4-yl]-propyl}-2-methyl-phenoxy)-2-methyl-propionic acid ethyl ester (0.065 g, 0.128 mmole) is treated with 3:1 MeOH/5.0N NaOH (4 mL) at room temperature overnight, and then concentrated. The resulting residue is diluted with water (2 mL), cooled down to 0° C., acidified to pH=2 by adding concentrated HCl dropwise. The aqueous suspension is loaded on a Chem elut tube and eluted with DCM (50 mL). Evaporation of methylene chloride gives the titled compound as an oil (0.060 g, 98%). Mass [EI+] 481 (M+H)+, [EI−] 479 (M−H)−.

後処理

  1. concentrationconcentrated
  2. additionThe resulting residue is diluted with water (2 mL)
  3. additionby adding concentrated HCl dropwise
  4. washeluted with DCM (50 mL)
  5. customEvaporation of methylene chloride

出典と根拠

ORDレコード
ord-16bc7c04ce9b40a4821aa1cb8ecb75d0
出典データセット
uspto-grants-2009_06
特許番号
US07544812B2

反応ノート

読み込み中…