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

HRID 361612노트

반응식

HRID 361612 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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%

후처리

  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

출처 및 근거

ORD 기록
ord-5c78a918d90a45fd82ec6dcd9951ca10
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05866594

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