Hydrochloric Acid → HCID 66847784、化合物

HRID 1631345ノート

反応式

HRID 1631345 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[C@@H:9]1[N:13]([C:14]2[CH:19]=[CH:18][N:17]3[N:20]=[CH:21][C:22]([C:23]([O:25]CC)=[O:24])=[C:16]3[N:15]=2)[C:12]([CH3:29])([CH3:28])[CH2:11][CH2:10]1.[OH-].[Na+].Cl>CO.[Cl-].[Na+].O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[C@@H:9]1[N:13]([C:14]2[CH:19]=[CH:18][N:17]3[N:20]=[CH:21][C:22]([C:23]([OH:25])=[O:24])=[C:16]3[N:15]=2)[C:12]([CH3:29])([CH3:28])[CH2:11][CH2:10]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86664571HCID 86664571、化合物

生成物 1

HCID 66847784HCID 66847784、化合物収率 97.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

(R)-ethyl 5-(5-(2,5-difluorophenyl)-2,2-dimethylpyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidine-3-carboxylate (136 mg, 0.340 mmol) was dissolved in MeOH (5.0 mL) and 1N NaOH (3.40 mL, 3.40 mmol) was added. The reaction was stirred at ambient temperature for 5 days and then heated at reflux for 4 hours. The reaction mixture was cooled, poured onto a mixture of brine (10 mL) and 2N HCl (5 mL) and extracted with DCM. The combined organic extracts were filtered through PS paper and concentrated to provide the title compound (123 mg, 97% yield) as a beige solid. MS (apci) m/z=373.0 (M+H).

後処理

  1. temperatureheated
  2. temperatureat reflux for 4 hours
  3. temperatureThe reaction mixture was cooled
  4. extractionextracted with DCM
  5. filtrationThe combined organic extracts were filtered through PS paper
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-350bd349b06542788116675342a75e2d
出典データセット
uspto-grants-2014_07
特許番号
US08791123B2

反応ノート

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