Diethyl Ether → (R)-2-azido-1-benzylethylamine

HRID 1057294ノート

反応式

HRID 1057294 の反応式
[N:1]([CH2:4][C@H:5]([NH:13]C(OC(C)(C)C)=O)[CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[N+:2]=[N-:3].CCOCC.[Na+].[Cl-]>Cl.C(O)C.O>[N:1]([CH2:4][C@H:5]([NH2:13])[CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)=[N+:2]=[N-:3]

参加物

7

反応物 3

HCID 3283Diethyl EtherHCID 5234Sodium ChlorideHCID 229417321-azido-2-(R)-(BOC-amino)-3-phenylpropane

生成物 1

HCID 14802497(R)-2-azido-1-benzylethylamine

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

The compound from step 3 (4.3 g, 15.6 mmol) is dissolved in 30 mL of 4 N HCl in ethanol, and the reaction mixture is stirred for 1.5 hours at room temperature. The solvent is stripped and chased with ether. The residue is dissolved in water, NaCl is added, and the mixture is extracted with ethyl ether, which is discarded. The aqueous layer is adjusted to pH 12 with K2CO3, saturated with NaCl, then extracted with CHCl3. The organic extract is washed with brine, dried (Na2SO4) and filtered. The solvent is removed under vacuum to afford the title compound.

後処理

  1. extractionthe mixture is extracted with ethyl ether, which
  2. extractionextracted with CHCl3
  3. extractionThe organic extract
  4. washis washed with brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customThe solvent is removed under vacuum

出典と根拠

ORDレコード
ord-0cbb3a2aa1644635bb4835f666288467
出典データセット
uspto-grants-2003_02
特許番号
US06514944B2

反応ノート

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