Hydrazine → 3-(Morpholine-4-sulfonyl)benzohydrazide

HRID 1777015

反応式

HRID 1777015 の反応式
[O:1]1[CH2:6][CH2:5][N:4]([S:7]([C:10]2[CH:11]=[C:12]([CH:17]=[CH:18][CH:19]=2)[C:13](OC)=[O:14])(=[O:9])=[O:8])[CH2:3][CH2:2]1.[NH2:20][NH2:21]>CO>[O:1]1[CH2:6][CH2:5][N:4]([S:7]([C:10]2[CH:11]=[C:12]([CH:17]=[CH:18][CH:19]=2)[C:13]([NH:20][NH2:21])=[O:14])(=[O:9])=[O:8])[CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 9321HydrazineHCID 779656Methyl 3-(morpholinosulfonyl)benzoate

生成物 1

HCID 8772463-(Morpholine-4-sulfonyl)benzohydrazide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

Methyl 3-(morpholinosulfonyl)benzoate (120 mg, 0.421 mmol) was added to hydrazine (17.52 mg, 0.547 mmol) in methanol and refluxed for 12 h at 65° C. The reaction was monitored by TLC. Upon completion of the reaction and cooling the reaction mixture, the solvent was removed by vacuum and then compound was purified by column chromatography to yield the title compound as an off white solid (90 mg). 1H NMR (400 MHz, CDCl3): δ 8.16 (m, 1H), 8.12 (m, 1H), 8.04 (m, 1H), 7.85 (m, 1H), 7.63 (t, 1H, J=8.0 Hz), 4.19 (m, 2H), 3.71 (m, 4H), 2.97 (m, 4H). ESI-MS: 286.1 [M+H]+.

後処理

  1. customUpon completion of the reaction
  2. temperaturecooling the reaction mixture
  3. customthe solvent was removed by vacuum
  4. customcompound was purified by column chromatography

出典と根拠

ORDレコード
ord-d13c493a79f245d6bfe9765152d75767
出典データセット
uspto-grants-2016_02
特許番号
US09266838B2

関連ノート

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