Triethylamine → N,N-Bis[2-(diethylamino)ethyl]-N'-(1-methylethyl)-N'-[2-(phenylsulfonyl)ethyl]urea

HRID 330419

反応式

HRID 330419 の反応式
[CH3:1][CH:2]([N:4]([CH2:8][CH2:9][S:10]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)(=[O:12])=[O:11])[C:5](Cl)=[O:6])[CH3:3].[CH2:19]([N:21]([CH2:32][CH3:33])[CH2:22][CH2:23][NH:24][CH2:25][CH2:26][N:27]([CH2:30][CH3:31])[CH2:28][CH3:29])[CH3:20].C(N(CC)CC)C>O1CCCC1.CCOCC>[CH2:30]([N:27]([CH2:28][CH3:29])[CH2:26][CH2:25][N:24]([CH2:23][CH2:22][N:21]([CH2:32][CH3:33])[CH2:19][CH3:20])[C:5]([N:4]([CH:2]([CH3:3])[CH3:1])[CH2:8][CH2:9][S:10]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)(=[O:12])=[O:11])=[O:6])[CH3:31]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 671541,2-Ethanediamine, N2-[2-(diethylamino)ethyl]-N1,N1-diethyl-HCID 13655164N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]carbamic chloride

生成物 1

HCID 14855301N,N-Bis[2-(diethylamino)ethyl]-N'-(1-methylethyl)-N'-[2-(phenylsulfonyl)ethyl]urea

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 7.67 g (0.0265 mole) of N-(1-methylethyl)-N-[2-(phenylsulfonyl)ethyl]carbamic chloride and 6.24 g (0.029 mole) of N'-[2-(diethylamino)ethyl]-N,N-diethyl-1,2-ethanediamine and 2.73 g (0.0270 mole) of triethylamine in 400 ml of tetrahydrofuran was refluxed for 6 hr and then was stirred at room temperature for 7 hr. The solvent was removed in vacuo and the residue was partitioned between methylene chloride and dilute sodium hydroxide. The methylene chloride solution was dried over sodium sulfate, and the solvent was removed in vacuo to give an oil. This was dissolved in ether, and the solution was extracted with three portions of water. The ether solution was dried over sodium sulfate, and the solvent was removed in vacuo to give an oil. This was pumped under high vacuum at 56° C. for 20 hr to give the title compound as an oil.

後処理

  1. temperaturewas refluxed for 6 hr
  2. customThe solvent was removed in vacuo
  3. customthe residue was partitioned between methylene chloride and dilute sodium hydroxide
  4. dry with materialThe methylene chloride solution was dried over sodium sulfate
  5. customthe solvent was removed in vacuo
  6. customto give an oil
  7. extractionthe solution was extracted with three portions of water
  8. dry with materialThe ether solution was dried over sodium sulfate
  9. customthe solvent was removed in vacuo
  10. customto give an oil
  11. waitThis was pumped under high vacuum at 56° C. for 20 hr

出典と根拠

ORDレコード
ord-279c13ebf324458dab675d5378c01dc5
出典データセット
uspto-grants-1990_01
特許番号
US04895840

関連ノート

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