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

HRID 454647노트

반응식

HRID 454647 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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]

출처 및 근거

ORD 기록
ord-4ee74432fd404c8c84f26d58b40856b4
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492582B2

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