Sodium Chloride → HCID 90387114、化合物

HRID 2170229ノート

反応式

HRID 2170229 の反応式
[O:1]=[C:2]([CH3:14])[CH2:3][C:4](ON1C(=O)CCC1=O)=[O:5].[CH3:15][O:16][C:17]1[CH:30]=[CH:29][C:20]([CH2:21][NH:22][CH2:23][CH2:24][C:25]([O:27][CH3:28])=[O:26])=[CH:19][CH:18]=1.C(N(CC)CC)C.[Cl-].[Na+]>ClCCl>[CH3:15][O:16][C:17]1[CH:18]=[CH:19][C:20]([CH2:21][N:22]([CH2:23][CH2:24][C:25]([O:27][CH3:28])=[O:26])[C:4](=[O:5])[CH2:3][C:2](=[O:1])[CH3:14])=[CH:29][CH:30]=1

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 8471TriethylamineHCID 5123089N-Hydroxysuccinimidyl acetoacetateHCID 12201326METHYL 3-(4-METHOXYBENZYLAMINO)PROPANOATE

生成物 1

HCID 90387114HCID 90387114、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A flask with stirbar was charged with 2,5-dioxopyrrolidin-1-yl 3-oxobutanoate (6.47 g, 32.5 mmol), methyl 3-(4-methoxybenzylamino)propanoate (prepared as described in Bew, S. et al, Chem Commun. 2006 (41), 4338-40, 7.7 g, 34.5 mmol) and triethylamine (5 mL, 35.9 mmol) in dichloromethane (125 mL). The solution was stirred overnight at ambient temperature, then shaken in a separatory funnel with saturated aqueous sodium chloride. The organics were then washed with saturated aqueous sodium chloride containing 0.1M HCl and dried over anhydrous sodium sulfate. Filtration and solvent removal provided the title compound.

後処理

  1. washThe organics were then washed with saturated aqueous sodium chloride containing 0.1M HCl
  2. dry with materialdried over anhydrous sodium sulfate
  3. filtrationFiltration and solvent removal

出典と根拠

ORDレコード
ord-29625289c34941ca9a8206d0743ae309
出典データセット
uspto-grants-2015_06
特許番号
US09050346B2

反応ノート

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