HRID32081

反应详情

EQUATION

反应方程式

HRID 32081 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(6-Formyl-1,2,3,4-tetrahydro-naphthalen-2-yl)-carbamic acid tert-butyl ester (Step D) (0.090 g, 0.33 mmol) was dissolved in N,N-dimethylacetamide (10 mL). Piperdine (0.162 mL, 1.63 mmol) was added and the mixture was stirred at RT for 30 min. NaBH(OAc)3 (0.173 g, 0.817 mmol) was added in one portion and the reaction was stirred at RT until complete consumption of starting material was observed by HPLC analysis. The reaction was in concentrated in vacuo and the residue was diluted with CH2Cl2 and H2O and the aqueous layer was made basic with NaOH. The layers were separated and the organics were dried over MgSO4 and concentrated in vacuo to afford the crude title compound, which was used without further purification. MS (APCI pos) 345 (M+H).

WORKUP

后处理

  1. stirringthe reaction was stirred at RT until complete consumption of starting material
  2. concentrationin concentrated in vacuo
  3. additionthe residue was diluted with CH2Cl2 and H2O
  4. customThe layers were separated
  5. dry with materialthe organics were dried over MgSO4
  6. concentrationconcentrated in vacuo