Acetic Anhydride → N-(6-bromo-2-methoxypyridin-3-yl)formamide

HRID 406318노트

반응식

HRID 406318 반응식
[C:1](OC(=O)C)(=[O:3])C.[Br:8][C:9]1[N:14]=[C:13]([O:15][CH3:16])[C:12]([NH2:17])=[CH:11][CH:10]=1>C(O)=O>[Br:8][C:9]1[N:14]=[C:13]([O:15][CH3:16])[C:12]([NH:17][CH:1]=[O:3])=[CH:11][CH:10]=1

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 105361376-Bromo-2-methoxypyridin-3-amine

생성물 1

HCID 71492501N-(6-bromo-2-methoxypyridin-3-yl)formamide

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

Acetic anhydride (203 mL) was added dropwise to formic acid (204 mL) under ice-cooling, and the mixture was stirred at the same temperature for 25 minutes. 6-Bromo-2-methoxypyridine-3-amine powder (CAS #89466-18-2, 146 g) was put into the reaction mixture over 10 minutes, and then the reaction solution was stirred at the same temperature for 30 minutes. The water bath was removed. tert-Butyl methyl ether (300 mL) and n-heptane (500 mL) were sequentially added dropwise to the reaction solution, and then the reaction solution was stirred for 30 minutes. The precipitated powder was collected by filtration. The resulting powder was crushed with a mortar, washed with tert-butyl methyl ether and then dried under reduced pressure to obtain 137.4 g of the title compound.

후처리

  1. temperaturecooling
  2. stirringthe reaction solution was stirred at the same temperature for 30 minutes
  3. customThe water bath was removed
  4. additiontert-Butyl methyl ether (300 mL) and n-heptane (500 mL) were sequentially added dropwise to the reaction solution
  5. stirringthe reaction solution was stirred for 30 minutes
  6. filtrationThe precipitated powder was collected by filtration
  7. customThe resulting powder was crushed with a mortar
  8. washwashed with tert-butyl methyl ether
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-885ca24e062e4198b06b71a83abe583a
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754100B2

반응 노트

불러오는 중…