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

HRID 1770051ノート

反応式

HRID 1770051 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9a269102a0694b1dbe9ae00c8240a19b
出典データセット
uspto-grants-1995_01
特許番号
US05384425

反応ノート

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