HRID29210

反应详情

EQUATION

反应方程式

HRID 29210 的结构方程式

PROCEDURE

实验过程

A mixture of tert-butyl (1S,2R)-1-benzyl-3-[(1-ethylpropoxy)amino]-2-hydroxypropylcarbamate (3.285 g, 8.98 mmol) and trifluoroacetic acid (25 mL) was stirred at ambient temperature under Argon for approximately 30 minutes. The reaction was evaporated in vacuo and the residue was partitioned between dichloromethane and aqueous sodium hydroxide (1N). The phases were separated and the aqueous phase was extracted with dichloromethane. The combined organic phases were dried over anhydrous sodium sulfate, filter, evaporated in vacuo and dried under high vacuum to provide (2R,3S)-3-amino-1-[(1-ethylpropoxy)amino]-4-phenyl-2-butanol (2.455 g, 100%) as a solid. H1-NMR (chloroform-D3): 0.94 (m, 6H), 1.56 (m, 4H), 2.55 (m, 1H), 3.01 (m, 2H), 3.22 (m, 2H), 3.51 (m, 1H), 3.81 (m, 1H), 7.30 (m, 5H). MS(ESI): 267(M+H).

WORKUP

后处理

  1. customThe reaction was evaporated in vacuo
  2. customthe residue was partitioned between dichloromethane and aqueous sodium hydroxide (1N)
  3. customThe phases were separated
  4. extractionthe aqueous phase was extracted with dichloromethane
  5. dry with materialThe combined organic phases were dried over anhydrous sodium sulfate
  6. filtrationfilter
  7. customevaporated in vacuo
  8. customdried under high vacuum