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

HRID 1057294

반응식

HRID 1057294 반응식
[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]

참가 물질

7

반응물 3

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

생성물 1

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

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0cbb3a2aa1644635bb4835f666288467
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06514944B2

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