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

HRID 361388

반응식

HRID 361388 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-benzylethylamine수율 78.9%

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매HCID 962Water용매

실험 절차

The compound from step 164c (4.3 g, 15.6 mmol) was dissolved in 30 mL of 4N HCl in ethanol, and the reaction mixture was stirred for 1.5 hours at room temperature. The solvent was stripped and chased with ether. The residue was dissolved in water, NaCl was added, and the mixture was extracted with ethyl ether, which was discarded. The aqueous layer was adjusted to pH 12 with K2CO3, saturated with NaCl, then extracted with CHCl3. The organic extract was washed with brine, dried (Na2SO4) and filtered. The solvent was removed under vacuum to afford 2.17 g of the title compound. MS m/z (M+H)+ : 177, MS m/z (M+NH4)+ : 194.

후처리

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

출처 및 근거

ORD 기록
ord-945ea424ab244a6187c5dfdeb60280c6
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05866549

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