Water → 6-Chloro-2-triphenylmethyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one

HRID 397573노트

반응식

HRID 397573 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[NH:9][N:10]=2)[N:7]=1.Cl[C:13]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C(N(C(C)C)C(C)C)C.O>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[N:9]([C:13]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)([C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=3)[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)[N:10]=2)[N:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6456Trityl chlorideHCID 81531DiisopropylethylamineHCID 64071826-chloro-2H,3H-[1,2,4]triazolo[4,3-b]pyridazin-3-one

생성물 1

HCID 230003076-Chloro-2-triphenylmethyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one수율 71.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

0.341 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one and 0.669 g of chlorotriphenylmethane were dissolved in 5 ml of N,N-dimethylformamide; 0.414 ml of N-ethyldiisopropylamine was added, followed by stirring at room temperature for 2 days. After water was added, the reaction mixture was extracted with ethyl acetate; the extract was washed with saline and dried over magnesium sulfate. After concentration under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with hexane-ethyl acetate (2:1). The desired fraction was collected and concentrated; the crystal obtained was collected by filtration, washed with diethyl ether, and dried, to yield 0.591 g of the title compound.

후처리

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washthe extract was washed with saline
  3. dry with materialdried over magnesium sulfate
  4. concentrationAfter concentration under reduced pressure
  5. washeluted with hexane-ethyl acetate (2:1)
  6. customThe desired fraction was collected
  7. concentrationconcentrated
  8. customthe crystal obtained
  9. filtrationwas collected by filtration
  10. washwashed with diethyl ether
  11. customdried

출처 및 근거

ORD 기록
ord-fbbef0e461ac4f1bafb5463b640ff18f
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610694B1

반응 노트

불러오는 중…