ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrochloric Acid → HCID 59208466、化合物

HRID 2243070
ノート
印刷プレビュー

反応式

HRID 2243070 の反応式
[H-].[Na+].[CH3:3][O:4][CH2:5][CH2:6][N:7]1[CH:11]=[CH:10][N:9]=[C:8]1[C:12](=[O:14])[CH3:13].Cl.C([O-])(O)=O.[Na+].[CH3:21][O:22][C:23](=O)[O:24]C>>[CH3:3][O:4][CH2:5][CH2:6][N:7]1[CH:11]=[CH:10][N:9]=[C:8]1[C:12](=[O:14])[CH2:13][C:23]([O:22][CH3:21])=[O:24]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 12021Dimethyl CarbonateHCID 24758Sodium hydrideHCID 516892Sodium BicarbonateHCID 59208500HCID 59208500、化合物2 回

生成物 1

HCID 59208466HCID 59208466、化合物

反応条件

温度
90 °C

実験手順

NaH (7.84 g, 196 mmol of a 60% dispersion in oil) was added portionwise to a solution of 6.18 g (Intermediate 57, 34.5 mmol) of 1-[1-(2-methoxyethyl)-1H-imidazol-2-yl]ethanone in 100 ml dimethylcarbonate. The mixture was heated to 90° C. for 2 hour forming a thick slurry. After cooling to room temperature, the mixture was slowly transferred to 1N HCl over ice. The mixture was brought to about pH 7 with NaHCO3, then saturated with NaCl and extracted 4 times with EtOAc. The EtOAc was dried over MgSO4, then concentrated to give an oil that was chromatographed on silica gel (100% DCM followed by gradient elution to 50% EtOAc in DCM) to yield the title compound. MS (ES) (M+H)+: 227 for C10H14N2O4; NMR: 3.18 (s, 3H), 3.61 (m, 5H), 4.07 (s, 2H), 4.52 (m, 2H), 7.24 (s, 1H), 7.61 (s, 1H).

後処理

  1. customforming a thick slurry
  2. temperatureAfter cooling to room temperature
  3. extractionsaturated with NaCl and extracted 4 times with EtOAc
  4. dry with materialThe EtOAc was dried over MgSO4
  5. concentrationconcentrated
  6. customto give an oil that
  7. customwas chromatographed on silica gel (100% DCM followed by gradient elution to 50% EtOAc in DCM)

出典と根拠

ORDレコード
ord-81bd22be8b7d4584bb7036c6f6280958
出典データセット
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07674801B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート