Phosphoric Acid → Zaleplon

HRID 1394391ノート

反応式

HRID 1394391 の反応式
C[N:2]([CH3:19])[CH:3]=[CH:4][C:5]([C:7]1[CH:8]=[C:9]([N:13]([CH2:17][CH3:18])[C:14](=[O:16])[CH3:15])[CH:10]=[CH:11][CH:12]=1)=O.N[C:21]1[C:25]([C:26]#[N:27])=C[NH:23][N:22]=1.P(=O)(O)(O)O>O.C(O)C>[CH3:18][CH2:17][N:13]([C:14]([CH3:15])=[O:16])[C:9]1[CH:10]=[CH:11][CH:12]=[C:7]([C:5]2[N:23]3[N:22]=[CH:21][C:25]([C:26]#[N:27])=[C:19]3[N:2]=[CH:3][CH:4]=2)[CH:8]=1

参加物

6

反応物 3

HCID 1004Phosphoric AcidHCID 53395302N-(3-(3-(Dimethylamino)-1-oxo-2-propenyl)phenyl)-N-ethylacetamideHCID 178510443HCID 178510443、化合物

生成物 1

HCID 5719Zaleplon収率 96.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

N-[3 -[3-(dimethylamino)-1-oxo-2-propenyl]phenyl]-N-ethylacetamide (2.6 g, 0.01 mol) and 3-amino-4-cyanopyrazole (1.08 g, 0.01 mol) were dissolved in the mixture of water (35 cm3) and ethanol (20 cm3). Phosphoric acid (85%) (0.67 cm3, 0.01 mol) was then added and the mixture was stirred at room temperature for about 8 hours. The reaction mixture was then cooled to about 5° C. and the crystalline product that formed was collected, washed with water and dried at about 60° C. to yield zaleplon (2.95 g, 96.7%) in 99.09% purity as determined by HPLC.

後処理

  1. temperatureThe reaction mixture was then cooled to about 5° C.
  2. customthe crystalline product that formed
  3. customwas collected
  4. washwashed with water
  5. customdried at about 60° C.

出典と根拠

ORDレコード
ord-cc0cb01d022f42c0835156bab2b080a1
出典データセット
uspto-grants-2008_03
特許番号
US07348429B2

反応ノート

読み込み中…