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

HRID 2407769ノート

反応式

HRID 2407769 の反応式
[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]

参加物

4

反応物 2

HCID 22985Ammonium nitrateHCID 12326832Ethyl 2-ethoxynicotinate

生成物 1

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

試薬・触媒・溶媒 1

HCID 9845Trifluoroacetic anhydride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-530e13399932498fa2da854c78a783b1
出典データセット
uspto-grants-2014_08
特許番号
US08809538B2

反応ノート

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