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Water → HCID 11435600、化合物

HRID 1374445
ノート
印刷プレビュー

反応式

HRID 1374445 の反応式
[NH2:1][C@@H:2]([CH3:8])[CH2:3][C:4]([O:6][CH3:7])=[O:5].Cl[C:10]([O:12][CH2:13][CH:14]=[CH2:15])=[O:11].C(N(C(C)C)CC)(C)C.O>C1COCC1>[CH2:13]([O:12][C:10]([NH:1][C@@H:2]([CH3:8])[CH2:3][C:4]([O:6][CH3:7])=[O:5])=[O:11])[CH:14]=[CH2:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 18052Allyl chloroformateHCID 81531DiisopropylethylamineHCID 9118386Methyl (3S)-3-aminobutanoate

生成物 1

HCID 11435600HCID 11435600、化合物収率 81.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of methyl (3S)-3-aminobutanoate (1.47 g, 12.5 mmol) in THF (30 ml) were added at 0° C. allyl chloroformate (1.60 ml, 15.1 mmol) and diisopropylethylamine (2.62 ml, 15.0 mmol), and the mixture was stirred at the same temperature for 30 minutes. The reaction mixture was poured into water and extracted twice with ethylacetate. The organic layer was washed with a saturated aqueous sodium chloride solution, was dried over magnesium sulfate and the organic solvent was removed under reduced pressure. The residue was purified by silica gel (25 g) chromatography to give methyl (3S)-3-{[(allyloxy)carbonyl]amino}butanoate (2.06 g, 81%).

後処理

  1. extractionextracted twice with ethylacetate
  2. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  3. dry with materialwas dried over magnesium sulfate
  4. customthe organic solvent was removed under reduced pressure
  5. customThe residue was purified by silica gel (25 g) chromatography

出典と根拠

ORDレコード
ord-0b850249c58948a6b09c13636a15a08a
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07163936B2

反応ノート

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