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3-Pyridinemethanol → {1-[3-(Pyridin-4-ylmethoxy)-pyrazin-2-yl]-pyrrolidin-3-yl}-carbamic acid tert-butyl ester

HRID 907562
ノート
印刷プレビュー

反応式

HRID 907562 の反応式
C[C:2](C)([O-:4])C.[K+].[CH:7]1[CH:12]=[N:11][CH:10]=[C:9](CO)[CH:8]=1.[C:15]([O:19][C:20](=[O:34])[NH:21][CH:22]1[CH2:26][CH2:25][N:24]([C:27]2[C:32](Cl)=[N:31][CH:30]=[CH:29][N:28]=2)[CH2:23]1)([CH3:18])([CH3:17])[CH3:16]>C(O)(C)(C)C>[C:15]([O:19][C:20](=[O:34])[NH:21][CH:22]1[CH2:26][CH2:25][N:24]([C:27]2[C:32]([O:4][CH2:2][C:8]3[CH:7]=[CH:12][N:11]=[CH:10][CH:9]=3)=[N:31][CH:30]=[CH:29][N:28]=2)[CH2:23]1)([CH3:18])([CH3:17])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 75103-PyridinemethanolHCID 23665647Potassium tert-butoxideHCID 59013776Tert-butyl (1-(3-chloropyrazin-2-yl)pyrrolidin-3-yl)carbamate

生成物 1

HCID 59013922{1-[3-(Pyridin-4-ylmethoxy)-pyrazin-2-yl]-pyrrolidin-3-yl}-carbamic acid tert-butyl ester収率 12%

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

To a round-bottom flask purged with N2 was charged with Potassium t-butoxide (7.6 g, 68.4 mmol) and t-butanol (140 mL). The mixture was flushed with N2 for approximately 5 min., while stirring. To this mixture was added pyridylcarbinol (7.4 g, 68.4 mmol), followed by [1-(3-chloro-pyrazin-2-yl)-pyrrolidin-3-yl]-carbamic acid tert-butyl ester (6.8 g, 22.8 mmol). The mixture was stirred at room temperature overnight. The mixture was concentrated in vacuo, and then diluted with water and extracted with EtOAc three times. The organic layer was washed with water and brine, dried over sodium sulfate, and then concentrated in vacuo. Purification of the crude by column chromatography afforded {1-[3-(pyridin-4-ylmethoxy)-pyrazin-2-yl]-pyrrolidin-3-yl}-carbamic acid tert-butyl ester (1 g, 12% yield).

後処理

  1. customTo a round-bottom flask purged with N2
  2. customThe mixture was flushed with N2 for approximately 5 min.
  3. stirringThe mixture was stirred at room temperature overnight
  4. concentrationThe mixture was concentrated in vacuo
  5. additiondiluted with water
  6. extractionextracted with EtOAc three times
  7. washThe organic layer was washed with water and brine
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated in vacuo
  10. customPurification of the crude by column chromatography

出典と根拠

ORDレコード
ord-7aa25689392242e8b40eb4a90e460fd8
出典データセット
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08013156B2

反応ノート

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