Sodium ethoxide → 6-Ethoxy-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine

HRID 657868

반응식

HRID 657868 반응식
Br.Cl[C:3]1[C:4]([CH3:14])=[C:5]([CH3:13])[C:6]2[N:7]([C:9]([NH2:12])=[N:10][N:11]=2)[N:8]=1.[O-:15][CH2:16][CH3:17].[Na+]>C(O)C>[CH2:16]([O:15][C:3]1[C:4]([CH3:14])=[C:5]([CH3:13])[C:6]2[N:7]([C:9]([NH2:12])=[N:10][N:11]=2)[N:8]=1)[CH3:17]

참가 물질

4

반응물 2

HCID 2723922Sodium ethoxideHCID 866507976-Chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide

생성물 1

HCID 580460056-Ethoxy-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine수율 108.9%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
60 °C

실험 절차

6-Chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.006; 4 g) were dissolved in ethanol (120 ml), admixed under argon with sodium ethoxide (5.86 g) and stirred at 60° C. for 1 h. Then the mixture was dried and the residue was purified using a 40 g silica gel cartridge (0-20% dichloromethane-ethanol gradient in 40 min). The clean product fractions were combined and dried. 3.24 g of the title compound were obtained, which still contained residual amounts of dichloromethane. LC-MS rt: 0.53 min [M+H]+: 208.1 (met. b)

후처리

  1. customThen the mixture was dried
  2. customthe residue was purified
  3. customa 40 g silica gel cartridge (0-20% dichloromethane-ethanol gradient in 40 min)
  4. customdried

출처 및 근거

ORD 기록
ord-474fb6ecf36e4e5f8d83674cfebd422c
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076336B2

연결된 노트

불러오는 중…