1,2-Ethanediamine, N1,N1,N2-trimethyl- → Tert-butyl 2-(5-(((2-(dimethylamino)ethyl)(methyl)amino)methyl)-2-(methoxymethoxy)benzamido)-4-phenylbenzoate

HRID 454647ノート

反応式

HRID 454647 の反応式
Br[CH2:2][C:3]1[CH:4]=[CH:5][C:6]([O:31][CH2:32][O:33][CH3:34])=[C:7]([CH:30]=1)[C:8]([NH:10][C:11]1[CH:23]=[C:22]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:21]=[CH:20][C:12]=1[C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])=[O:9].[CH3:35][N:36]([CH3:41])[CH2:37][CH2:38][NH:39][CH3:40]>CC(C)=O>[CH3:35][N:36]([CH3:41])[CH2:37][CH2:38][N:39]([CH2:2][C:3]1[CH:4]=[CH:5][C:6]([O:31][CH2:32][O:33][CH3:34])=[C:7]([CH:30]=1)[C:8]([NH:10][C:11]1[CH:23]=[C:22]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:21]=[CH:20][C:12]=1[C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])=[O:9])[CH3:40]

参加物

4

反応物 2

HCID 673381,2-Ethanediamine, N1,N1,N2-trimethyl-HCID 66990849Tert-butyl 2-(5-(bromomethyl)-2-(methoxymethoxy)benzamido)-4-phenylbenzoate

生成物 1

HCID 66991111Tert-butyl 2-(5-(((2-(dimethylamino)ethyl)(methyl)amino)methyl)-2-(methoxymethoxy)benzamido)-4-phenylbenzoate

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Under ice-cooling, tert-butyl 2-(5-(bromomethyl)-2-(methoxymethoxy)benzamido)-4-phenylbenzoate (0.12 g) was added to an acetone (1.8 mL) solution of N,N,N′-trimethylethylenediamine (0.089 mL), followed by stirring at room temperature for 1 hour. The solvent was evaporated under reduced pressure, and a saturated aqueous solution of sodium bicarbonate and chloroform were added to the residue. The organic layer was separated and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography [eluent: 100-90% chloroform/methanol] to obtain 0.070 g of tert-butyl 2-(5-(((2-(dimethylamino)ethyl)(methyl)amino)methyl)-2-(methoxymethoxy)benzamido)-4-phenylbenzoate.

後処理

  1. temperatureUnder ice-cooling
  2. customThe solvent was evaporated under reduced pressure
  3. additiona saturated aqueous solution of sodium bicarbonate and chloroform were added to the residue
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography [eluent: 100-90% chloroform/methanol]

出典と根拠

ORDレコード
ord-4ee74432fd404c8c84f26d58b40856b4
出典データセット
uspto-grants-2013_07
特許番号
US08492582B2

反応ノート

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