Diazomethane diethylether → Methyl 4-chloro-3,7-dimethylindole-2-carboxylate

HRID 361612

反応式

HRID 361612 の反応式
[N+](=[CH2:3])=[N-].CCOCC.[Cl:9][C:10]1[CH:18]=[CH:17][C:16]([CH3:19])=[C:15]2[C:11]=1[C:12]([CH3:23])=[C:13]([C:20]([OH:22])=[O:21])[NH:14]2>CCOCC>[Cl:9][C:10]1[CH:18]=[CH:17][C:16]([CH3:19])=[C:15]2[C:11]=1[C:12]([CH3:23])=[C:13]([C:20]([O:22][CH3:3])=[O:21])[NH:14]2

参加物

4

反応物 2

HCID 21186548Diazomethane diethyletherHCID 541380234-Chloro-3,7-dimethylindole-2-carboxylic acid

生成物 1

HCID 54167277Methyl 4-chloro-3,7-dimethylindole-2-carboxylate収率 77%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

An excess diazomethane ether solution was added to an ether solution of 0.50 g (2.24 mmol) of 4-chloro-3,7-dimethylindole-2-carboxylic acid under ice-cooling. The reaction mixture was allowed to stand for 30 minutes and then washed with 1N HCl aqueous solution and aqueous saturated sodium chloride solution. The ether layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to provide white crystals. The crude crystals were purified by silica gel column chromatography to provide 0.41 g of white crystals. Yield: 77%

後処理

  1. temperaturecooling
  2. washwashed with 1N HCl aqueous solution and aqueous saturated sodium chloride solution
  3. dry with materialThe ether layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto provide white crystals
  6. customThe crude crystals were purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-5c78a918d90a45fd82ec6dcd9951ca10
出典データセット
uspto-grants-1999_02
特許番号
US05866594

関連ノート

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