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Lithium aluminum hydride → (1R,3S,4S)-2-azabicyclo(2.2.1)heptan-3-ylmethanol

HRID 60251
ノート
印刷プレビュー

反応式

HRID 60251 の反応式
Cl.[C@H:2]12[CH2:8][C@H:5]([CH2:6][CH2:7]1)[C@@H:4]([C:9](O)=[O:10])[NH:3]2.[AlH4-].[Li+]>O1CCCC1>[C@H:2]12[CH2:8][C@H:5]([CH2:6][CH2:7]1)[C@@H:4]([CH2:9][OH:10])[NH:3]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 28112Lithium aluminum hydrideHCID 20849996(1R,3S,4S)-2-azabicyclo[2.2.1]heptane-3-carboxylic acid hydrochloride

生成物 1

HCID 11480448(1R,3S,4S)-2-azabicyclo(2.2.1)heptan-3-ylmethanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a slurry of (1R,3S,4S)-2-azabicyclo[2.2.1]heptane-3-carboxylic acid hydrogen chloride (500 mg, 3 mmol) in tetrahydrofuran (4.6 mL) was added lithium tetrahydroaluminate (1N solution in tetrahydrofuran, 5.7 mL, 6 mmol) dropwise over 10 minutes. The reaction mixture was stirred overnight at ambient temperature under an atmosphere of nitrogen. The reaction was quenched with a few drops of water, diluted with diethyl ether (50 mL) and tetrahydrofuran (25 mL). The reaction mixture was basified to a pH of ˜11 by the addition of potassium hydroxide pellets and then stirred vigorously for 30 minutes. The reaction mixture was filtered over sodium sulfate, concentrated in vacuo, redissolved in methylene chloride (10 mL), dried once more over sodium sulfate, filtered, and concentrated in vacuo to afford a yellow crystalline solid, which was used in the next step without any further purification (400 mg, 100%).

後処理

  1. customThe reaction was quenched with a few drops of water
  2. additiondiluted with diethyl ether (50 mL) and tetrahydrofuran (25 mL)
  3. additionThe reaction mixture was basified to a pH of ˜11 by the addition of potassium hydroxide pellets
  4. stirringstirred vigorously for 30 minutes
  5. filtrationThe reaction mixture was filtered over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. dissolutionredissolved in methylene chloride (10 mL)
  8. dry with materialdried once more over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo
  11. customto afford a yellow crystalline solid, which
  12. customwas used in the next step without any further purification (400 mg, 100%)

出典と根拠

ORDレコード
ord-8c2b4dbc37494cfb83c23da8bfe60101
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09440976B2

反応ノート

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