Phosphoric Acid → Zaleplon

HRID 1394390노트

반응식

HRID 1394390 반응식
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.CO>[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

참가 물질

6

반응물 3

HCID 1004Phosphoric AcidHCID 53395302N-(3-(3-(Dimethylamino)-1-oxo-2-propenyl)phenyl)-N-ethylacetamideHCID 178510443HCID 178510443, 화합물

생성물 1

HCID 5719Zaleplon수율 91.5%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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 methanol (20 cm3). Phosphoric acid (85%) (0.67 cm3, 0.01 mol) was then added and the mixture was stirred at room temperature for about 4 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 (2.79 g, 91.5%) in 98.83% purity as determined by HPLC.

후처리

  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.

출처 및 근거

ORD 기록
ord-aeb53de75d6e447b8b4896a3a55b9239
출처 데이터셋
uspto-grants-2008_03
특허 번호
US07348429B2

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