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Methanesulfonyl chloride → HCID 86681621、化合物

HRID 571209
ノート
印刷プレビュー

反応式

HRID 571209 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH2:11][C:12]([O:14][CH3:15])=[O:13])[CH:6]=[CH:5]2.[CH3:16][S:17](Cl)(=[O:19])=[O:18]>N1C=CC=CC=1>[CH3:16][S:17]([NH:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH2:11][C:12]([O:14][CH3:15])=[O:13])[CH:6]=[CH:5]2)(=[O:19])=[O:18]
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 31297Methanesulfonyl chlorideHCID 43165394Methyl 2-(5-amino-1H-indol-1-yl)acetate

生成物 1

HCID 86681621HCID 86681621、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of methyl 2-(5-amino-1H-indol-1-yl)acetate (730 mg, 3.54 mmol) in pyridine (15 ml), methanesulfonyl chloride (418 μl, 5.36 mmol) was added, and the mixture was reacted for 2 hours at room temperature. The solvent was evaporated and the resulting crude was partitioned between 1N HCl and ethyl acetate; the aqueous phase was extracted with ethyl acetate (3×30 ml) and dried over sodium sulfate. The solvent was removed obtaining crude methyl 2-(5-(methylsulfonamido)-1H-indol-1-yl)acetate that was used in the next step without any additional purification (1 g, 3.54 mmol, quantitative yield). MS/ESI+ 283.3 [MH]+.

後処理

  1. customthe mixture was reacted for 2 hours at room temperature
  2. customThe solvent was evaporated
  3. customthe resulting crude was partitioned between 1N HCl and ethyl acetate
  4. extractionthe aqueous phase was extracted with ethyl acetate (3×30 ml)
  5. dry with materialdried over sodium sulfate
  6. customThe solvent was removed

出典と根拠

ORDレコード
ord-1fa3df13da0c4a9d9a6176260c0ccabf
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09024027B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート