Tetrahydrofuran → HCID 12150401、化合物

HRID 275730ノート

反応式

HRID 275730 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 12150401HCID 12150401、化合物収率 76.8%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
130 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1cd8c7108340447786d3b330e00ac02b
出典データセット
uspto-grants-2002_03
特許番号
US06352989B1

反応ノート

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