4-Chloro-6-nitroquinazoline → N-[3-chloro-4-(2-pyridylmethoxy)phenyl]-6-nitro-quinazolin-4-amine

HRID 2199343ノート

反応式

HRID 2199343 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[CH:10]=2)[N:5]=[CH:4][N:3]=1.[Cl:15][C:16]1[CH:17]=[C:18]([CH:20]=[CH:21][C:22]=1[O:23][CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=1)[NH2:19]>C(O)(C)C>[Cl:15][C:16]1[CH:17]=[C:18]([NH:19][C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[C:9]([N+:12]([O-:14])=[O:13])[CH:10]=3)[N:5]=[CH:4][N:3]=2)[CH:20]=[CH:21][C:22]=1[O:23][CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=1

参加物

4

反応物 2

HCID 113562574-Chloro-6-nitroquinazolineHCID 167812123-Chloro-4-(2-pyridylmethoxy)aniline

生成物 1

HCID 18967699N-[3-chloro-4-(2-pyridylmethoxy)phenyl]-6-nitro-quinazolin-4-amine収率 74.8%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

4-Chloro-6-nitro-quinazoline 4b crude product (6.06 g, 28.90 mmol) was dissolved in 100 mL of isopropanol, followed by addition of 3-chloro-4-(2-pyridylmethoxy)aniline 4c (7.47 g, 31.8 mmol). The reaction mixture was heated to reflux for 5 hours. The mixture was cooled to room temperature, the solid was precipitated, filtered and the filter cake was washed with ethyl acetate, saturated brine (50 mL) and water (150 mL) successively, dried under vacuum to obtain the title compound N-[3-chloro-4-(2-pyridylmethoxy)phenyl]-6-nitro-quinazolin-4-amine 4d (8.38 g, yield 74.8%) as a yellow solid.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 5 hours
  3. customthe solid was precipitated
  4. filtrationfiltered
  5. washthe filter cake was washed with ethyl acetate, saturated brine (50 mL) and water (150 mL) successively
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-3d45d870d25541c0a10c6a14edcd3ebd
出典データセット
uspto-grants-2016_06
特許番号
US09358227B2

反応ノート

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