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

HRID 2239543
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HRID 2239543 반응식
[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]
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참가 물질

4

반응물 2

HCID 80182-MethoxyethylamineHCID 74740Phenylmethanesulfonyl chloride

생성물 1

HCID 4467329N-(2-methoxyethyl)-1-phenylmethanesulfonamide수율 99.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-60be09b87bf34ee68b8021ef90f6750c
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07723333B2

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