Acetonitrile → 3-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide

HRID 2243767

반응식

HRID 2243767 반응식
O[O:2][S:3]([O-:5])=O.[K+].[F:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([F:14])[C:9]=1[N:15]1[C:20]2[N:21]=[C:22](SC)[N:23]=[C:24]([C:25]3[CH:26]=[C:27]([CH:34]=[CH:35][C:36]=3[CH3:37])[C:28]([NH:30][CH2:31][CH2:32][CH3:33])=[O:29])[C:19]=2[CH2:18][NH:17][C:16]1=[O:40].[C:41](#N)C>O>[F:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([F:14])[C:9]=1[N:15]1[C:20]2[N:21]=[C:22]([S:3]([CH3:41])(=[O:5])=[O:2])[N:23]=[C:24]([C:25]3[CH:26]=[C:27]([CH:34]=[CH:35][C:36]=3[CH3:37])[C:28]([NH:30][CH2:31][CH2:32][CH3:33])=[O:29])[C:19]=2[CH2:18][NH:17][C:16]1=[O:40]

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 119502633-[8-(2,6-difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamideHCID 23707502Potassium hydroxy sulfite

생성물 1

HCID 592079903-[8-(2,6-difluorophenyl)-2-(methylsulfonyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirring suspension of Oxone (817.96 g, 1.33 mole, 3 eq) in water (2142 mL, 10 vol) was added 3-[8-(2,6-difluorophenyl)-2-(methylthio)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-propylbenzamide (214.21 g 0.443 mole, 1 eq) suspended in acetonitrile (4284 mL). The resulting mixture was stirred at ambient temperature overnight. The mixture was then filtered and the residue stirred sequentially with 5% sodium metabisulfite (2×3000 mL) and water (1×300 mL). The filtrate from the reaction mixture was then diluted with water (2142 mL, 10 vol). The solid that formed was then collected by filtration. The solid was washed well with water then dried at the pump to yield the title compound. LC-MS m/z 516 (M+H)+, 2.77 min (ret time). It was used without further purification although corresponding sulfoxide was present (about 10%).

후처리

  1. filtrationThe mixture was then filtered
  2. stirringthe residue stirred sequentially with 5% sodium metabisulfite (2×3000 mL) and water (1×300 mL)
  3. additionThe filtrate from the reaction mixture was then diluted with water (2142 mL, 10 vol)
  4. customThe solid that formed
  5. filtrationwas then collected by filtration
  6. washThe solid was washed well with water
  7. customthen dried at the pump

출처 및 근거

ORD 기록
ord-76886ac03f234014bb68a8eca88cfe8d
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07674789B2

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