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

HRID 132424

反応式

HRID 132424 の反応式
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

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-b566f640e1a0409aaf8a2f2fb9542367
出典データセット
uspto-grants-2008_06
特許番号
US07384931B2

関連ノート

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