Water → HCID 18509409、化合物

HRID 1356810ノート

反応式

HRID 1356810 の反応式
[CH3:1][C:2]([CH3:23])([CH3:22])[C:3]#[C:4]/[CH:5]=[CH:6]/[CH2:7][N:8]([CH2:10][C:11]1[CH:12]=[C:13]([C:18](O)([CH3:20])[CH3:19])[CH:14]=[CH:15][C:16]=1[CH3:17])[CH3:9].P(Cl)(Cl)(Cl)=O.O.[OH-].[Na+]>N1C=CC=CC=1>[CH3:1][C:2]([CH3:23])([CH3:22])[C:3]#[C:4]/[CH:5]=[CH:6]/[CH2:7][N:8]([CH2:10][C:11]1[CH:12]=[C:13]([C:18]([CH3:20])=[CH2:19])[CH:14]=[CH:15][C:16]=1[CH3:17])[CH3:9]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 18509459HCID 18509459、化合物

生成物 1

HCID 18509409HCID 18509409、化合物収率 85.7%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
135 °C

実験手順

Compound 33 (520 mg; 1.66 mmol) was dissolved in pyridine (6 ml), and phosphorus oxychloride (1.27 g; 8.3 mmol) was added thereto. The mixture was stirred for 1 hour at 130-140° C., and then cooled. The reaction mixture was poured into water, and alkalinized with sodium hydroxide pellet. The mixture was extracted with ether (120 ml), and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1), to thereby yield 420 mg of the target compound (yield: 85.7%).

後処理

  1. temperaturecooled
  2. extractionThe mixture was extracted with ether (120 ml)
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=20:1)

出典と根拠

ORDレコード
ord-b8a87f0af27742d1bf7aa592ca0f257b
出典データセット
uspto-grants-2003_07
特許番号
US06586633B1

反応ノート

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