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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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m-Chloroperbenzoic acid → 2-(4-{[(3,4-Dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)-N-methoxy-6-(methylsulfonyl)isonicotinamide

HRID 2233977
ノート
印刷プレビュー

反応式

HRID 2233977 の反応式
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([CH3:8])[NH:4][C:3]=1[C:9]([NH:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]2[CH:19]=[C:20]([CH:26]=[C:27]([S:29]([CH3:31])=[O:30])[N:28]=2)[C:21]([NH:23][O:24][CH3:25])=[O:22])[CH2:14][CH2:13]1)=[O:10].C1C=C(Cl)C=C(C(OO)=[O:40])C=1>C(Cl)Cl>[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([CH3:8])[NH:4][C:3]=1[C:9]([NH:11][CH:12]1[CH2:13][CH2:14][N:15]([C:18]2[CH:19]=[C:20]([CH:26]=[C:27]([S:29]([CH3:31])(=[O:40])=[O:30])[N:28]=2)[C:21]([NH:23][O:24][CH3:25])=[O:22])[CH2:16][CH2:17]1)=[O:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 866083232-(4-{[(3,4-Dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)-N-methoxy-6-(methylsulfinyl)isonicotinamide

生成物 1

HCID 112029112-(4-{[(3,4-Dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)-N-methoxy-6-(methylsulfonyl)isonicotinamide収率 11.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-(4-{[(3,4-Dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)-N-methoxy-6-(methylsulfinyl)isonicotinamide (Example 152) (90 mg, 0.185 mmol) was dissolved in anhydrous DCM (5 ml). mCPBA (32 mg, 0185 mmol) was added and the mixture was stirred at room temperature for 12 h. The crude mixture was diluted and washed with 10% sodium thiosulfate, water, brine and dried over sodium sulfate and concentrated in vacuo. The brown oil was purified by flash chromatography eluting with acetonitrile/water (0.1% TFA) to give the title compound (11 mg).

後処理

  1. washwashed with 10% sodium thiosulfate, water, brine
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customThe brown oil was purified by flash chromatography
  5. washeluting with acetonitrile/water (0.1% TFA)

出典と根拠

ORDレコード
ord-237cfaf1f049413dbc3247154b7c9501
出典データセット
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07709503B2

反応ノート

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