m-Chloroperbenzoic acid → HCID 67400511、化合物

HRID 471575ノート

反応式

HRID 471575 の反応式
[S:1]([NH:5][C:6]1[CH:13]=[CH:12][CH:11]=[C:10]([S:14][CH3:15])[C:7]=1[C:8]#[N:9])(=[O:4])(=[O:3])[NH2:2].C1C=C(Cl)C=C(C(OO)=[O:24])C=1>ClCCl>[S:1]([NH:5][C:6]1[CH:13]=[CH:12][CH:11]=[C:10]([S:14]([CH3:15])=[O:24])[C:7]=1[C:8]#[N:9])(=[O:3])(=[O:4])[NH2:2]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 67400359HCID 67400359、化合物

生成物 1

HCID 67400511HCID 67400511、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The mixture of 2-sulfamoylamino-6-(methylthio)benzonitrile (Example 104a) (48 mg, 0.2 mmol) and MCPBA (69 mg, 0.4 mmol) in dichloromethane (16 mL) was heated refluxed overnight. After cooling down, the precipitation was collected by filtration, rinsed with dichloromethane, dried in the air to give the title compound. 1H NMR (400 MHz, DMSO-d6) δ 2.83 (s, 3H), 7.35 (brs, 2H), 7.72-6.69 (m, 2H), 7.92 (t, J=8.0 Hz, 1H), 9.87 (brs, 1H).

後処理

  1. temperaturewas heated
  2. temperaturerefluxed overnight
  3. temperatureAfter cooling down
  4. customthe precipitation
  5. filtrationwas collected by filtration
  6. washrinsed with dichloromethane
  7. customdried in the air

出典と根拠

ORDレコード
ord-741907e5e3124b75b0c41e025ae2a1c3
出典データセット
uspto-grants-2014_01
特許番号
US08633186B2

反応ノート

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