ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1,1'-Carbonyldiimidazole → N-[2-(Diethylamino)ethyl]-N-(1-methylethyl)-N'-[2-(phenylsulfonyl)ethyl]urea

HRID 745193
ノート
印刷プレビュー

反応式

HRID 745193 の反応式
[C:1]1([S:7]([CH2:10][CH2:11][NH2:12])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:13](N1C=CN=C1)(N1C=CN=C1)=[O:14].[CH2:25]([N:27]([CH2:34][CH3:35])[CH2:28][CH2:29][NH:30][CH:31]([CH3:33])[CH3:32])[CH3:26]>O1CCCC1>[CH2:34]([N:27]([CH2:25][CH3:26])[CH2:28][CH2:29][N:30]([CH:31]([CH3:33])[CH3:32])[C:13]([NH:12][CH2:11][CH2:10][S:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)(=[O:8])=[O:9])=[O:14])[CH3:35]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 682631,1'-CarbonyldiimidazoleHCID 35454972-(Benzenesulfonyl)ethan-1-amineHCID 12639037Diethyl((2-((propan-2-yl)amino)ethyl))amine

生成物 1

HCID 20152862N-[2-(Diethylamino)ethyl]-N-(1-methylethyl)-N'-[2-(phenylsulfonyl)ethyl]urea

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A mixture of 6.96 g (0.0376 mole) of 2-phenylsulfonylethanamine and 6.64 g (0.041 mole) of 1,1'-carbonyldiimidazole in 400 ml of tetrahydrofuran was stirred at room temperature for 1 hr. A solution of 6.16 g (0.039 mole) of N-[2-(diethylamino)ethyl]-2-propanamine in 50 ml of tetrahydrofuran was added, and the mixture was refluxed for 13 hr. The solvent was removed in vacuo, and the residue was dissolved in a 50/50 mixture of ether and methylene chloride. The solution was extracted with water and was dried over magnesium sulfate. The solvent was removed in vacuo to give an oil. Flash chromatography on silica gel (methanol) gave 5.74 g (41.36%) of clear, colorless oil: 1H NMR (CDCl3)δ8.5 (br s, 1, NH) 7.46-8.05 (m, 5, aromatic), 4.45 (m, 1, (CH3)2CH), 3.48 (br s, 4, SO2CH2CH 2), 3.0 (t, 2, (CH2CH2N-Et2) 2.3-2.8 (m, 6, CH2N CH2N(CH2CH3)2), 0.90-1.2 (m, 12, CH3 groups).

後処理

  1. temperaturethe mixture was refluxed for 13 hr
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in a 50/50 mixture of ether and methylene chloride
  4. extractionThe solution was extracted with water
  5. dry with materialwas dried over magnesium sulfate
  6. customThe solvent was removed in vacuo
  7. customto give an oil
  8. customFlash chromatography on silica gel (methanol) gave 5.74 g (41.36%) of clear, colorless oil

出典と根拠

ORDレコード
ord-0a0c049c547b4c5a88247500ca4f1e1e
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04597902

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート