Sulfuric Acid → HCID 21873976, 화합물

HRID 985080노트

반응식

HRID 985080 반응식
[NH2:1][C:2]1[C:3]2[N:4]([C:17]([CH3:21])=[C:18]([CH3:20])[N:19]=2)[CH:5]=[CH:6][C:7]=1[C:8](=[O:16])[CH:9]=[CH:10][C:11]1[CH:15]=[CH:14][S:13][CH:12]=1.S(=O)(=O)(O)O.[OH-].[Na+]>>[CH3:20][C:18]1[N:19]=[C:3]2[C:2]3[NH:1][CH:10]([C:11]4[CH:15]=[CH:14][S:13][CH:12]=4)[CH2:9][C:8](=[O:16])[C:7]=3[CH:6]=[CH:5][N:4]2[C:17]=1[CH3:21]

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 69586325HCID 69586325, 화합물

생성물 1

HCID 21873976HCID 21873976, 화합물수율 69.2%

실험 절차

2.6 g of 8-amino-2,3-dimethyl-7-[3-(3-thienyl)-1-oxo-2-propenyl]imidazo[1,2-a]pyridine are treated at room temperature with 20 ml of aqueous 70% strength sulfuric acid, poured onto ice water (100 ml) after 90 minutes, neutralized with aqueous 6 N sodium hydroxide solution and extracted three times with 50 ml of methylene chloride each time. The combined organic phases are washed with water, dried over sodium sulfate, the solvent is stripped off in vacuo and the remaining yellow oil is stirred with 15 ml of diethyl ether. The yellowish solid obtained here is filtered off and dried in vacuo. 1.8 g of the title compound of m.p. 176-77° C. (diethyl ether) are obtained.

후처리

  1. additionpoured onto ice water (100 ml) after 90 minutes
  2. extractionextracted three times with 50 ml of methylene chloride each time
  3. washThe combined organic phases are washed with water
  4. dry with materialdried over sodium sulfate
  5. customThe yellowish solid obtained here
  6. filtrationis filtered off
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-e566304a11bd4b63bc1faf0c835d369d
출처 데이터셋
uspto-grants-2005_03
특허 번호
US06869949B2

반응 노트

불러오는 중…