Methanol → Methyl 3-(morpholinosulfonyl)benzoate

HRID 1777014

反応式

HRID 1777014 の反応式
[O:1]1[CH2:6][CH2:5][N:4]([S:7]([C:10]2[CH:11]=[C:12]([CH:16]=[CH:17][CH:18]=2)[C:13]([OH:15])=[O:14])(=[O:9])=[O:8])[CH2:3][CH2:2]1.OS(O)(=O)=O.[CH3:24]O>>[O:1]1[CH2:6][CH2:5][N:4]([S:7]([C:10]2[CH:11]=[C:12]([CH:16]=[CH:17][CH:18]=2)[C:13]([O:15][CH3:24])=[O:14])(=[O:9])=[O:8])[CH2:3][CH2:2]1

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 2574763-(Morpholine-4-sulfonyl)benzoic acid

生成物 1

HCID 779656Methyl 3-(morpholinosulfonyl)benzoate

実験手順

3-(Morpholinosulfonyl)benzoic acid (100 mg, 0.369 mmol) was refluxed overnight in methanol in the presence of catalytic concentrated H2SO4 at 65° C. The reaction was monitored by TLC. After completion of the reaction, the solvent was removed by vacuum and then compound was purified by column chromatography to yield the title compound as an off white solid (60 mg). 1H NMR (400 MHz, CDCl3): δ 8.38 (t, 1H, J=1.6 Hz), 8.27 (m, 1H), 7.92 (m, 1H), 7.64 (t, 1H, J=8.0 Hz), 3.95 (s, 3H), 3.73 (m, 4H), 3.00 (m, 4H). ESI-MS: 286.1 [M+H]+.

後処理

  1. customAfter completion of the reaction
  2. customthe solvent was removed by vacuum
  3. customcompound was purified by column chromatography

出典と根拠

ORDレコード
ord-3e9c3a7dc800445ca5232c80f16a5d1c
出典データセット
uspto-grants-2016_02
特許番号
US09266838B2

関連ノート

読み込み中…