Sodium hydride → 4-Methoxy-2-(3-methyl-1,2,4-oxadiazol-5-yl)benzenamine

HRID 53244

반응식

HRID 53244 반응식
[H-].[Na+].[C:3](=[N:6][OH:7])([NH2:5])[CH3:4].[NH2:8][C:9]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:10]=1[C:11](OC)=O>O1CCCC1>[CH3:20][O:19][C:16]1[CH:17]=[CH:18][C:9]([NH2:8])=[C:10]([C:11]2[O:7][N:6]=[C:3]([CH3:4])[N:5]=2)[CH:15]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 30926N-HydroxyacetamidineHCID 13052275Methyl 2-amino-5-methoxybenzoate

생성물 1

HCID 199621234-Methoxy-2-(3-methyl-1,2,4-oxadiazol-5-yl)benzenamine수율 72.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Sodium hydride (594 mg) was added to a stirred suspension of acetamide oxime (1.0 g) and 4 molecular sieves (4 g) in dry tetrahydrofuran (50 ml) under nitrogen. The mixture was heated at 60° for 30 min then allowed to cool to room temperature. A solution of 2-amino-5-methoxybenzoic acid, methyl ester (2.0 g) in dry tetrahydrofuran (20 ml) was added and the mixture stirred at reflux for 2.5 h. The suspension was allowed to cool, filtered and the filtrate evaporated to give the title compound as a yellow solid (1.64 g)

후처리

  1. temperatureThe mixture was heated at 60° for 30 min
  2. temperatureat reflux for 2.5 h
  3. temperatureto cool
  4. filtrationfiltered
  5. customthe filtrate evaporated

출처 및 근거

ORD 기록
ord-de14df84f908491bba4e59f0038f2dee
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05618827

연결된 노트

불러오는 중…