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

Sodium Bicarbonate → 3,4-Diethoxycarbonyl-2-fluoro-5-nitro-6-phenylpyridine

HRID 37492
노트
인쇄 미리보기

반응식

HRID 37492 반응식
N[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:5]([N+:18]([O-:20])=[O:19])=[C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[N:3]=1.B(F)(F)[F:28].F.N([O-])=O.[Na+].C(=O)([O-])O.[Na+]>C(O)(=O)C.O>[CH2:11]([O:10][C:8]([C:7]1[C:2]([F:28])=[N:3][C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[C:5]([N+:18]([O-:20])=[O:19])[C:6]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[O:9])[CH3:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 516892Sodium BicarbonateHCID 9855450Trifluoroborane HydrofluorideHCID 199356032-Amino-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridineHCID 23668193Sodium Nitrite

생성물 1

HCID 199356173,4-Diethoxycarbonyl-2-fluoro-5-nitro-6-phenylpyridine

시약·촉매·용매 2

HCID 176
Acetic Acid
용매
HCID 962Water용매

반응 조건

온도
-5 °C

실험 절차

In 2 ml of acetic acid was dissolved 100 mg of 2-amino-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine, and 1.5 ml of 42% hydrofluoroboric acid was added to the solution. The mixture was cooled to -5° C., followed by adding dropwise a solution of 21 mg (1.1 eq) of sodium nitrite dissolved in 0.5 ml of water. Thirty minutes later, the temperature of the mixture was elevated to room temperature and the mixture was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. After the organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. After the solvent was distilled off, the resulting crystals (2-pyridone compound) were collected by filtration with hexane, and washed. The solvent was distilled off from the obtained filtrate, to give an oily substance.

후처리

  1. additionwas added to the solution
  2. customThirty minutes
  3. customwas elevated to room temperature
  4. extractionfollowed by extraction with ethyl acetate
  5. washAfter the organic layer was washed with water
  6. dry with materiala saturated aqueous solution of sodium chloride, and dried
  7. distillationAfter the solvent was distilled off
  8. filtrationthe resulting crystals (2-pyridone compound) were collected by filtration with hexane
  9. washwashed
  10. distillationThe solvent was distilled off from the obtained filtrate
  11. customto give an oily substance

출처 및 근거

ORD 기록
ord-4afe1d8998b646889314d45135528e41
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05420275

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트