Tetrahydrofuran → HCID 12150401, 화합물

HRID 275730노트

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HRID 275730 반응식
Cl[C:2]1[N:11]=[C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[CH:13]=2)[C:9]2[C:4](=[CH:5][C:6]([O:23][CH3:24])=[C:7]([O:21][CH3:22])[CH:8]=2)[N:3]=1.[CH2:25]([N:27](CC)CC)C.C(OCC)(=O)C.O1CCCC1>CN1CCCC1=O>[CH3:22][O:21][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][C:6]=1[O:23][CH3:24])[N:3]=[C:2]([NH:27][CH3:25])[N:11]=[C:10]2[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[CH:13]=1

참가 물질

6

반응물 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 121503982-Chloro-6,7-dimethoxy-4-(3-nitrophenyl)quinazoline

생성물 1

HCID 12150401HCID 12150401, 화합물수율 76.8%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

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온도
130 °C

실험 절차

2.50 g of 2-chloro-6,7-dimethoxy-4-(3-nitrophenyl)quinazoline obtained in Production Example 1,4.89 g methylamine hydrochloride and 11.0 g triethylamine were suspended in 25 ml 1-methyl-2-pyrrolidinone and stirred at 130° C. for 18 hours in a sealed tube. Ethyl acetate and tetrahydrofuran were added thereto, and the reaction solution was washed with water 5 times and then with brine and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the crude product was purified and separated by silica gel column chromatography (hexane:ethyl acetate=1:2). The product was recrystallized from tetrahydrofuran-ethyl acetate to give 1.89 g of the title compound as yellow crystals.

후처리

  1. washthe reaction solution was washed with water 5 times
  2. dry with materialwith brine and dried over anhydrous magnesium sulfate
  3. customThe solvent was evaporated
  4. customthe crude product was purified
  5. customseparated by silica gel column chromatography (hexane:ethyl acetate=1:2)
  6. customThe product was recrystallized from tetrahydrofuran-ethyl acetate

출처 및 근거

ORD 기록
ord-1cd8c7108340447786d3b330e00ac02b
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06352989B1

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