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

HRID 1762187노트

반응식

HRID 1762187 반응식
[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

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fa560c57532a489b988757d53d396939
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04831041

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