Ammonium Hydroxide → HCID 57467466、化合物

HRID 1890793ノート

反応式

HRID 1890793 の反応式
[F:1][C:2]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:3]=1[O:4][C:5]([CH3:10])([CH3:9])[C:6](O)=[O:7].CC[N:18]=C=NCCCN(C)C.Cl.[OH-].[NH4+]>C(Cl)Cl>[F:1][C:2]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:3]=1[O:4][C:5]([CH3:10])([CH3:9])[C:6]([NH2:18])=[O:7]

参加物

5

反応物 3

HCID 14923Ammonium HydroxideHCID 15318012-(2,4-Difluorophenoxy)-2-methylpropanoic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 57467466HCID 57467466、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-(2,4-difluorophenoxy)-2-methylpropanoic acid (10.0 g, 46.3 mmol, Chembridge) in methylene chloride (200 mL) were added 1-hydroxybenzotriaole hydrate (8.5 g, 55.5 mmol, Aldrich), N-(3-dimethylaminopropyl)-N-ethylcarbodimide hydrochloride (10.6 g, 55.5 mmol, Aldrich) and ammonium hydroxide (54.0 g, 463 mmol). The reaction mixture was stirred at room temperature for 16 hours and then quenched with water (100 mL). The aqueous layer was extracted with methylene chloride (3×100 mL). The combined organic extracts were washed with brine, 5% citric acid, and brine (100 mL each), dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to obtain the titled compound. MS (ESI+) m/z 233 (M+NH4)+.

後処理

  1. customquenched with water (100 mL)
  2. extractionThe aqueous layer was extracted with methylene chloride (3×100 mL)
  3. washThe combined organic extracts were washed with brine, 5% citric acid, and brine (100 mL each)
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-e9bcaedc02ed4d96ab6dbe1cce32478d
出典データセット
uspto-grants-2013_08
特許番号
US08507493B2

反応ノート

読み込み中…