Ammonium Chloride → 2-Amino-3-(2-methoxycarbonylamino-6-methylbenzyloxy)pyridine

HRID 1762187ノート

反応式

HRID 1762187 の反応式
[Cl-].[NH4+].[CH3:3][O:4][C:5]([NH:7][C:8]1[CH:24]=[CH:23][CH:22]=[C:21]([CH3:25])[C:9]=1[CH2:10][O:11][C:12]1[C:13]([N+:18]([O-])=O)=[N:14][CH:15]=[CH:16][CH:17]=1)=[O:6]>O.C(O)C.[Fe]>[NH2:18][C:13]1[C:12]([O:11][CH2:10][C:9]2[C:21]([CH3:25])=[CH:22][CH:23]=[CH:24][C:8]=2[NH:7][C:5]([O:4][CH3:3])=[O:6])=[CH:17][CH:16]=[CH:15][N:14]=1

参加物

6

反応物 2

HCID 25517Ammonium ChlorideHCID 143684013-(2-Methoxycarbonylamino-6-methylbenzyloxy)-2-nitropyridine

生成物 1

HCID 200425332-Amino-3-(2-methoxycarbonylamino-6-methylbenzyloxy)pyridine

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a mixture of iron powder (2.76 g) and ammonium chloride (0.275 g) in water (19 ml) and ethanol (63 ml) was added portionwise 3-(2-methoxycarbonylamino-6-methylbenzyloxy)-2-nitropyridine (6.27 g) under reflux and then stirred for an additional 30 minutes. The hot mixture was filtered by suction and the filtrate was made alkaline with sodium bicarbonate and evaporated in vacuo. The residue was washed with water, dried, and recrystallized from ethyl acetate to give 2-amino-3-(2-methoxycarbonylamino-6-methylbenzyloxy)pyridine.

後処理

  1. temperatureunder reflux
  2. filtrationThe hot mixture was filtered by suction
  3. customevaporated in vacuo
  4. washThe residue was washed with water
  5. customdried
  6. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-fa560c57532a489b988757d53d396939
出典データセット
uspto-grants-1989_05
特許番号
US04831041

反応ノート

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