反应 #640541

ord-501ce0d1c1b34300aeecdb837887f482

反应方程式

Nc1ccc(C(=O)O)cn1
6-aminonicotinic acid
CCO
ethanol
CCOC(=O)c1ccc(N)nc1
white solid
CCOC(=O)c1ccc(N)nc1
Ethyl 6-Aminonicotinate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他was bubbled in dry hydrochloric acid at 0° C.
  2. 2
    温度the solution was refluxed until all the solids
  3. 3
    workup.DISSOLUTIONdissolved
  4. 4
    其他The solvents were removed under reduced pressure
  5. 5
    workup.DISSOLUTIONthe residue dissolved in ethyl acetate
  6. 6
    洗涤washed with saturated sodium bicarbonate, brine
  7. 7
    浓缩concentrated

实验过程

To a suspension of 1.3 g (9.4 mmol) 6-aminonicotinic acid in 100 mL of ethanol, was bubbled in dry hydrochloric acid at 0° C., then the solution was refluxed until all the solids dissolved. The solvents were removed under reduced pressure, the residue dissolved in ethyl acetate, washed with saturated sodium bicarbonate, brine and concentrated to afford 1.37 g of a white solid, m/e=166(M+H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE042889E1uspto-grants-2011_11