m-Chloroperbenzoic acid → HCID 67400511、化合物

HRID 711712ノート

反応式

HRID 711712 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-d4acf21124534927996937eaf6263efc
出典データセット
uspto-grants-2015_11
特許番号
US09181276B2

反応ノート

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