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2-Methoxyethylamine → N-(2-methoxyethyl)-1-phenylmethanesulfonamide

HRID 2239543
ノート
印刷プレビュー

反応式

HRID 2239543 の反応式
[C:1]1([CH2:7][S:8](Cl)(=[O:10])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:12][O:13][CH2:14][CH2:15][NH2:16]>C1COCC1>[CH3:12][O:13][CH2:14][CH2:15][NH:16][S:8]([CH2:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)(=[O:10])=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 80182-MethoxyethylamineHCID 74740Phenylmethanesulfonyl chloride

生成物 1

HCID 4467329N-(2-methoxyethyl)-1-phenylmethanesulfonamide収率 99.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Phenylmethanesulfonyl chloride (3.0 g, 15.7 mmol) was dissolved in dry THF (15 mL) and it was added dropwise to a solution of 2-methoxyethylamine (2.36 g, 31.5 mmol) in dry THF (50 mL) at 0° C. After addition the ice-bath was removed and the reaction was stirred at rt for 2.5 h. The solvent was removed in vacuo and the residue was dissolved in DCM. The mixture was washed with one portion of 5% aqueous HCl, several portions of water, dried through a phase separator and evaporated to give the title compound (3.58 g, 94%); 1H NMR (400 MHz, CDCl3): δ 7.43-7.35 (m, 5H), 4.52 (br s, 1H), 4.26 (s, 2H), 3.40 (t, 2H), 3.32 (s, 3H), 3.14-3.09 (m, 2H); Mass Spectrum: M−H+ 228.

後処理

  1. customwas removed
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in DCM
  4. washThe mixture was washed with one portion of 5% aqueous HCl, several portions of water
  5. customdried through a phase separator
  6. customevaporated

出典と根拠

ORDレコード
ord-60be09b87bf34ee68b8021ef90f6750c
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07723333B2

反応ノート

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