Potassium Carbonate → 4-(3-t-butylureidomethyl)-1-(N-heptylaminomethyl)benzene

HRID 1770051노트

반응식

HRID 1770051 반응식
[C:1]([NH:5][C:6](=[O:17])[NH:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][NH2:16])=[CH:11][CH:10]=1)([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].I[CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31]>CN(C)C=O>[C:1]([NH:5][C:6](=[O:17])[NH:7][CH2:8][C:9]1[CH:10]=[CH:11][C:12]([CH2:15][NH:16][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])=[CH:13][CH:14]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 202741-IodoheptaneHCID 200967404-(3-t-Butylureidomethyl)-1-aminomethylbenzene

생성물 1

HCID 200967264-(3-t-butylureidomethyl)-1-(N-heptylaminomethyl)benzene수율 47.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 0.97 g 4-(3-t-butylureidomethyl)-1-aminomethylbenzene obtained in Example 8, 0.57 g anhydrous potassium carbonate and 20 ml dimethylformamide was stirred at room temperature for 30 minutes, 0.93 g 1-iodoheptane was added, and stirring was continued at room temperature for an additional three hours. After distilling off the solvent under reduced pressure, the residue was extracted with chloroform, and the extract was washed with water. The chloroform was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography, giving 0.65 g of 4-(3-t-butylureidomethyl)-1-(N-heptylaminomethyl)benzene.

후처리

  1. stirringstirring
  2. waitwas continued at room temperature for an additional three hours
  3. distillationAfter distilling off the solvent under reduced pressure
  4. extractionthe residue was extracted with chloroform
  5. washthe extract was washed with water
  6. distillationThe chloroform was distilled off under reduced pressure
  7. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-9a269102a0694b1dbe9ae00c8240a19b
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05384425

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