Ammonium nitrate → 3-Pyridinecarboxylic acid, 2-ethoxy-5-nitro-, ethyl ester

HRID 2407769노트

반응식

HRID 2407769 반응식
[N+:1]([O-:4])([O-])=[O:2].[NH4+].[CH2:6]([O:8][C:9]1[N:19]=[CH:18][CH:17]=[CH:16][C:10]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH3:7]>FC(F)(F)C(OC(=O)C(F)(F)F)=O>[CH2:6]([O:8][C:9]1[N:19]=[CH:18][C:17]([N+:1]([O-:4])=[O:2])=[CH:16][C:10]=1[C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH3:7]

참가 물질

4

반응물 2

HCID 22985Ammonium nitrateHCID 12326832Ethyl 2-ethoxynicotinate

생성물 1

HCID 104442903-Pyridinecarboxylic acid, 2-ethoxy-5-nitro-, ethyl ester수율 56.3%

시약·촉매·용매 1

HCID 9845Trifluoroacetic anhydride용매

실험 절차

Ammonium nitrate (1.11 g) was added portionwise to an ice-cooled solution of the compound prepared in Example 285 (0.900 g) in trifluoroacetic anhydride (11.5 mL). The mixture was stirred at room temperature overnight and then carefully poured into ice-water and the resulting suspension stirred for an hour. The precipitate was collected by filtration and washed with water. The solids were dried under vacuo to obtain the title compound (0.624 g) having the following physical data.

후처리

  1. stirringthe resulting suspension stirred for an hour
  2. filtrationThe precipitate was collected by filtration
  3. washwashed with water
  4. customThe solids were dried under vacuo

출처 및 근거

ORD 기록
ord-530e13399932498fa2da854c78a783b1
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809538B2

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