Water → 4-Allylamino-6-nitro-2-[2-(piperidinocarbonyl)ethylamino]quinazoline

HRID 1250604ノート

反応式

HRID 1250604 の反応式
[CH2:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([N+:15]([O-:17])=[O:16])[CH:13]=2)[N:8]=[C:7](Cl)[N:6]=1)[CH:2]=[CH2:3].Cl.[N:20]1([C:26]([CH2:28][CH2:29][NH2:30])=[O:27])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1.C(N(CC)CC)C.O>C(#N)C>[CH2:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([N+:15]([O-:17])=[O:16])[CH:13]=2)[N:8]=[C:7]([NH:30][CH2:29][CH2:28][C:26]([N:20]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]2)=[O:27])[N:6]=1)[CH:2]=[CH2:3]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 177503443-Amino-1-(piperidin-1-yl)propan-1-one hydrochlorideHCID 183264874-Allylamino-2-chloro-6-nitroquinazoline

生成物 1

HCID 183265474-Allylamino-6-nitro-2-[2-(piperidinocarbonyl)ethylamino]quinazoline収率 87.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

150 mg (0.57 mmol) of 4-allylamino-2-chloro-6-nitroquinazoline was dissolved in 10 ml of acetonitrile, and then 220 mg (1.14 mmol) of 2-piperidinocarbonylethylamine hydrochloride and 0.40 ml (2.85 mmol) of triethylamine were added thereto, followed by heating under reflux overnight. To the reaction solution was added water, followed by extraction with ethyl acetate, washing with brine and drying over anhydrous sodium sulfate. After the solvent was distilled off, the residue was purified by a silica gel column to give 191 mg (87.7%) of the title compound.

後処理

  1. temperatureby heating
  2. temperatureunder reflux overnight
  3. extractionfollowed by extraction with ethyl acetate
  4. washwashing with brine
  5. dry with materialdrying over anhydrous sodium sulfate
  6. distillationAfter the solvent was distilled off
  7. customthe residue was purified by a silica gel column

出典と根拠

ORDレコード
ord-d13ea15565794d88ab9a2961f944eb54
出典データセット
uspto-grants-2002_01
特許番号
US06339089B2

反応ノート

読み込み中…