Methanol → Methyl 3-(morpholinosulfonyl)benzoate

HRID 877599

反応式

HRID 877599 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-44c5d39c81284701a3faf3cdebbfc980
出典データセット
uspto-grants-2015_03
特許番号
US08987335B2

関連ノート

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