Potassium Carbonate → (S)-7-(2-hydroxyethyl)-9-neopentyl-6,7,9,10-tetrahydroazepino[3,4-e]indazol-8(3H)-one

HRID 1985472

반응식

HRID 1985472 반응식
C([O:4][CH2:5][CH2:6][C@H:7]1[C:20](=[O:21])[N:19]([CH2:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:18][C:10]2[C:11]3[CH:12]=[N:13][NH:14][C:15]=3[CH:16]=[CH:17][C:9]=2[CH2:8]1)(=O)C.C(=O)([O-])[O-].[K+].[K+]>CO>[OH:4][CH2:5][CH2:6][C@H:7]1[C:20](=[O:21])[N:19]([CH2:22][C:23]([CH3:26])([CH3:25])[CH3:24])[CH2:18][C:10]2[C:11]3[CH:12]=[N:13][NH:14][C:15]=3[CH:16]=[CH:17][C:9]=2[CH2:8]1

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 59731999(S)-2-(9-neopentyl-8-oxo-3,6,7,8,9,10-hexahydroazepino[3,4-e]indazol-7-yl)ethyl acetate

생성물 1

HCID 59731990(S)-7-(2-hydroxyethyl)-9-neopentyl-6,7,9,10-tetrahydroazepino[3,4-e]indazol-8(3H)-one수율 94%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

(S)-2-(9-neopentyl-8-oxo-3,6,7,8,9,10-hexahydroazepino[3,4-e]indazol-7-yl)ethyl acetate (18 mg, 0.05 mmol) was dissolved in methanol (1 mL). Potassium carbonate (20 mg, 0.14 mmol) was added to the mixture. Reaction stirred at room temperature for 1 hour. Amberlite IRC-50 ion exchange resin was added to the mixture. Reaction stirred at room temperature for 15 minutes. Mixture was filtered. Filtrate was concentrated in vacuo. The title compound was obtained as yellow residue in 94% yield. MS m/e (M+H)+=316.

후처리

  1. customReaction
  2. additionAmberlite IRC-50 ion exchange resin was added to the mixture
  3. customReaction
  4. stirringstirred at room temperature for 15 minutes
  5. filtrationMixture was filtered
  6. concentrationFiltrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-cbe9d695fae5494587e1cf387f14ea32
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07544680B2

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