HCID 22097096, 화합물 → HCID 22097212, 화합물

HRID 1458841노트

반응식

HRID 1458841 반응식
Cl[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[N+:12]([O-])=O)[N:8]([CH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1)[C:7](=[O:21])[C:6](=[O:22])[NH:5]2>O1CCCC1.CO.CN(C)C=O.[Pd]>[NH2:12][C:11]1[CH:10]=[C:9]2[C:4]([NH:5][C:6](=[O:22])[C:7](=[O:21])[N:8]2[CH:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]2)=[CH:3][CH:2]=1

참가 물질

4

반응물 1

HCID 22097096HCID 22097096, 화합물

생성물 1

HCID 22097212HCID 22097212, 화합물수율 80.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 86634690HCID 86634690, 화합물용매

실험 절차

28.9 g (89 mmol) of 6-Chloro-1-cyclohexyl-7-nitro-2,3(1H,4H)-quinoxalinedione were dissolved in 300 ml of tetrahydrofuran/methanol/dimethylformamide (3:3:1) and, after addition of 3 g of palladium/carbon (10%), hydrogenated. The mixture was filtered, the carbon was washed with methanolic ammonia solution, and the combined filtrates were concentrated under reduced pressure. The residue was chromatographed on silica gel with the mobile phase toluene/acetone/glacial acetic acid (10:10:1) to yield 2.2 g (8%) of product e1and 18.5 g (80%) of product e2.

후처리

  1. filtrationThe mixture was filtered
  2. washthe carbon was washed with methanolic ammonia solution
  3. concentrationthe combined filtrates were concentrated under reduced pressure
  4. customThe residue was chromatographed on silica gel with the mobile phase toluene/acetone/glacial acetic acid (10:10:1)

출처 및 근거

ORD 기록
ord-e86df05639174b0f8a007f27d01d076f
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05852017

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