HRID451775

反应详情

EQUATION

反应方程式

HRID 451775 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(S)-tert-butyl 1-amino-3-cyclohexyl-2-methyl-1-oxopropan-2-ylcarbamate To a solution of (S)-tert-butyl 1-amino-3-cyclohexyl-2-methyl-1-oxopropan-2-ylcarbamate (811 mg, 2.85 mmol) in anhydrous toluene (15 mL) at 0° C. was added Red-Al (65%, 2.66 g, 2.6 mL, 8.55 mmol) within 20 min. After the addition, the reaction was allowed to be stirred at room temperature overnight. The reaction was cooled to 0° C. and quenched with Na2SO4.10H2O. The resulting mixture was stirred for 2-3 h, filtered through Celite, and washed with THF (200 mL). The filtrate was dried and concentrated to give crude product (S)-tert-butyl 1-cyclohexyl-3-(ethylamino)propan-2-ylcarbamate (860 mg). MS ESI +ve m/z 271 (M+H).

WORKUP

后处理

  1. additionAfter the addition
  2. temperatureThe reaction was cooled to 0° C.
  3. customquenched with Na2SO4.10H2O
  4. stirringThe resulting mixture was stirred for 2-3 h
  5. filtrationfiltered through Celite
  6. washwashed with THF (200 mL)
  7. customThe filtrate was dried
  8. concentrationconcentrated