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Triethylsilane → (S)-2-amino-4,4-difluoro-pentanoic acid methyl ester

HRID 19309
ノート
印刷プレビュー

反応式

HRID 19309 の反応式
[CH3:1][O:2][C:3](=[O:21])[C@@H:4]([NH:10]C(OCC1C=CC=CC=1)=O)[CH2:5][C:6]([F:9])([F:8])[CH3:7].C([SiH](CC)CC)C>[Pd].CO>[CH3:1][O:2][C:3](=[O:21])[C@@H:4]([NH2:10])[CH2:5][C:6]([F:9])([F:8])[CH3:7]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 12052Triethylsilane3 回HCID 57535380HCID 57535380、化合物

生成物 1

HCID 57946221(S)-2-amino-4,4-difluoro-pentanoic acid methyl ester収率 43.4%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒3 回HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

In a flask under argon was placed (S)-2-benzyloxycarbonylamino-4,4-difluoro-pentanoic acid methyl ester (626 mg, 2.08 mmol), methanol (8 mL) and 10% palladium on activated carbon (100 mg). Triethylsilane (3 mL) was added slowly and the mixture stirred at 25° C. for 30 min. Another portion of 10% palladium on activated carbon (100 mg) and triethylsilane (3 mL) was added and the mixture was stirred for 30 min. A third portion of 10% palladium on activated carbon (100 mg) and triethylsilane (3 mL) was added and the mixture was stirred for 30 min. The mixture was filtered to remove the catalyst and the solids washed with methanol. The filterate was concentrated in vacuo, azeotroped with toluene, dissolved in dichloromethane and concentrated in vacuo with silica gel (2 g). Purification by Biotage flash chromatography (Aspire 40 g column, 100% ethyl acetate) afforded (S)-2-amino-4,4-difluoro-pentanoic acid methyl ester (151 mg) as a clear colorless liquid.

後処理

  1. customIn a flask under argon was placed
  2. stirringthe mixture was stirred for 30 min
  3. stirringthe mixture was stirred for 30 min
  4. filtrationThe mixture was filtered
  5. customto remove the catalyst
  6. washthe solids washed with methanol
  7. concentrationThe filterate was concentrated in vacuo
  8. customazeotroped with toluene
  9. dissolutiondissolved in dichloromethane
  10. concentrationconcentrated in vacuo with silica gel (2 g)
  11. customPurification by Biotage flash chromatography (Aspire 40 g column, 100% ethyl acetate)

出典と根拠

ORDレコード
ord-a5f207c3c18646ceb932bfd46a4ee98e
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07741327B2

反応ノート

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