홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Nitric Acid → 3-Methyl-5-nitro-2-pyridone

HRID 598077
노트
인쇄 미리보기

반응식

HRID 598077 반응식
[CH3:1][C:2]1[C:3](N)=[N:4][CH:5]=[CH:6][CH:7]=1.[N+:9]([O-])([OH:11])=[O:10].[OH2:13]>S(=O)(=O)(O)O>[CH3:1][C:2]1[C:3](=[O:13])[NH:4][CH:5]=[C:6]([N+:9]([O-:11])=[O:10])[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 944Nitric Acid2회HCID 962WaterHCID 153472-Amino-3-methylpyridine

생성물 1

HCID 890973-Methyl-5-nitro-2-pyridone수율 35%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매2회

반응 조건

온도
30 °C

실험 절차

A solution of (3-methylpyridin-2-yl)amine (10 g, 90 mmol) in 50 ml of concentrated sulfuric acid was cooled to 5° C. in ice-salt bath. A mixture of 7 ml each of concentrated sulfuric acid and concentrated nitric acid was added slowly with stirring while maintaining the reaction temperature below 10° C. This mixture was then allowed to warm to 30° C. overnight. The solution was stirred rapidly while 7 ml of concentrated nitric acid was added at such a rate as to keep the temperature below 40° C. Approximately 10 ml of the solution was then poured into 20 ml of water and heated to 100° C.; large quantities of gas were evolved. When gas evolution ceased, the remainder of the nitrating mixture was added in 10 ml portions with heating. When the last of the nitrating mixture had been added, the solution was cooled rapidly by placing the flask in an ice bath and by adding ice directly to the solution. The light brown precipitate was filtered and dried to afford 5.0 g (35%) of the title compound.

후처리

  1. additionwas added slowly
  2. temperaturewhile maintaining the reaction temperature below 10° C
  3. additionwas added at such a rate as
  4. customthe temperature below 40° C
  5. temperatureheated to 100° C.
  6. additionthe remainder of the nitrating mixture was added in 10 ml portions
  7. temperaturewith heating
  8. additionWhen the last of the nitrating mixture had been added
  9. temperaturethe solution was cooled rapidly
  10. additionby adding ice directly to the solution
  11. filtrationThe light brown precipitate was filtered
  12. customdried

출처 및 근거

ORD 기록
ord-d44484b6abd342f4b4a40f3ae0c0f490
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07897607B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트