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Water → 2-Tert-butoxy-8-nitro-3,6,7-trichloroquinoxaline

HRID 1060574
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HRID 1060574 반응식
[N+:1]([C:4]1[C:13]([Cl:14])=[C:12]([Cl:15])[CH:11]=[C:10]2[C:5]=1[N:6]=[C:7](Cl)[C:8]([Cl:16])=[N:9]2)([O-:3])=[O:2].[CH3:18][C:19]([CH3:22])([O-:21])[CH3:20].[K+].C1(C)C=CC=CC=1.O>C(O)(C)(C)C>[C:19]([O:21][C:7]1[C:8]([Cl:16])=[N:9][C:10]2[C:5](=[C:4]([N+:1]([O-:3])=[O:2])[C:13]([Cl:14])=[C:12]([Cl:15])[CH:11]=2)[N:6]=1)([CH3:22])([CH3:20])[CH3:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 1140TolueneHCID 107575382,3,6,7-Tetrachloro-5-nitro-quinoxalineHCID 23665647Potassium tert-butoxide

생성물 1

HCID 186291982-Tert-butoxy-8-nitro-3,6,7-trichloroquinoxaline수율 60.6%

시약·촉매·용매 1

HCID 6386tert-Butanol
용매

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온도
0 °C

실험 절차

To 5-nitro-2,3,6,7-tetrachloroquinoxaline 1608 mg obtained in Example 7(1), was added dropwise a solution of potassium tert-butoxide 644 mg in tert-butanol (15 mL) at −5 to 0° C. The reaction mixture was stirred at 0° C. for 30 min, and toluene 50 mL, 0.1 M sodium dihydrogen phosphate 5 mL, and water were added thereto with shaking. The organic layer was separated, washed with water and saturated saline, and dried over MgSO4. After evaporation, the residue was subjected to column chromato (silica gel/toluene) and crystallized from acetone, to give the title compound (colorless crystal) 1092 mg.

후처리

  1. stirringwith shaking
  2. customThe organic layer was separated
  3. washwashed with water and saturated saline
  4. dry with materialdried over MgSO4
  5. customAfter evaporation
  6. customcrystallized from acetone

출처 및 근거

ORD 기록
ord-478288073e6241509b41fd8c4ac649e5
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06525054B1

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