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Methane → Azd-0156

HRID 1486920
ノート
印刷プレビュー

反応式

HRID 1486920 の反応式
Br[C:2]1[CH:11]=[CH:10][C:9]2[N:8]=[CH:7][C:6]3[N:12]([CH3:22])[C:13](=[O:21])[N:14]([CH:15]4[CH2:20][CH2:19][O:18][CH2:17][CH2:16]4)[C:5]=3[C:4]=2[CH:3]=1.C([O-])([O-])=O.[K+].[K+].[CH3:29][N:30]([CH3:50])[CH2:31][CH2:32][CH2:33][O:34][C:35]1[CH:40]=[CH:39][C:38](B2OC(C)(C)C(C)(C)O2)=[CH:37][N:36]=1.C>CCO>[CH3:50][N:30]([CH3:29])[CH2:31][CH2:32][CH2:33][O:34][C:35]1[N:36]=[CH:37][C:38]([C:2]2[CH:11]=[CH:10][C:9]3[N:8]=[CH:7][C:6]4[N:12]([CH3:22])[C:13](=[O:21])[N:14]([CH:15]5[CH2:20][CH2:19][O:18][CH2:17][CH2:16]5)[C:5]=4[C:4]=3[CH:3]=2)=[CH:39][CH:40]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 297MethaneHCID 11430Potassium CarbonateHCID 17998906N,N-Dimethyl-3-((5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-yl)oxy)propan-1-amineHCID 1185234078-bromo-3-methyl-1-(tetrahydro-2H-pyran-4-yl)-1,3-dihydro-2H-imidazo[4,5-c]quinolin-2-one

生成物 1

HCID 118502708Azd-0156収率 93.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
78.5 °C

実験手順

On a larger scale, 8-bromo-3-methyl-1-(oxan-4-yl)imidazo[5,4-c]quinolin-2-one (1700.1 g) was suspended in EtOH (20.4 L) in a 50 L vessel then K2CO3 (1948.7 g) and N,N-dimethyl-3-[5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-yl]oxypropan-1-amine (1731.4 g) added. EtOH (6.8 L) and purified water (5.1 L) were added to the mixture followed by the addition chloro(2-dicyclohexylphosphino-2′,4′,6′-triisopropyl-1,1′-biphenyl)[2-(2′-amino-1,1′-biphenyl)]palladium(II) (37.3 g). The mixture was heated to reflux (77-80° C.) and stirred for 30 mins at reflux then cooled to 20° C. prior to being distilled under reduced pressure to a volume of 12.6 L. The batch was then cooled to 15-25° C. and purified water (19.9 L) added. The batch was stirred for 1 h 5 mins, filtered and the filter cake washed with purified water (3×3.7 L) then dried under vacuum at 40° C. to afford crude desired material (1978 g, 91.3%). The reaction was repeated on a similar scale to deliver a further 2084 g of crude material. The purification of the crude 8-[6-(3-dimethylaminopropoxy)pyridin-3-yl]-3-methyl-1-(oxan-4-yl)imidazo[5,4-c]quinolin-2-one (2066.9 g) was carried out in 6 portions of 350 g or less. Crude 8-[6-(3-dimethylaminopropoxy)pyridin-3-yl]-3-methyl-1-(oxan-4-yl)imidazo[5,4-c]quinolin-2-one (350.1 g) was charged to a 10 L flask with EtOH (7.7 L) and heated until a solution was formed (68-73° C.). Activated charcoal (35 g) was added and the solution stirred at 70-75° C. for 1 h. The hot solution was filtered using a porosity 3 sinter funnel through a celite pad (˜40 g) in small portions to ensure the product stayed in solution. The celite pad was washed with hot EtOH (2 L) to remove any residual product, on the celite and the initial filtrate charged to the vessel and the wash filtrate was stored in a carboy. This process was repeated with the remaining portions of crude material. After completion of the 6 hot titrations carried out over 2 days the filtrate in the vessel was distilled under reduced pressure until the remaining filtrate (held in a carboy) could be added. The batch was then heated until a solution was formed (69° C.) and the distillation was then continued until the volume in the vessel was equal to 5 volumes of the input material (maximum distillation batch temperature=55° C.). The distillation was stopped and the batch cooled to 5-15° C., filtered, washed with EtOH (2.3 L) and dried to give the pure desired product (1926 g, 93.2% yield).

後処理

  1. customEtOH (6.8 L) and purified water (5.1 L)
  2. additionwere added to the mixture
  3. additionfollowed by the addition chloro(2-dicyclohexylphosphino-2′,4′,6′-triisopropyl-1,1′-biphenyl)[2-(2′-amino-1,1′-biphenyl)]palladium(II) (37.3 g)
  4. temperatureThe mixture was heated
  5. temperatureat reflux
  6. temperaturethen cooled to 20° C.
  7. distillationto being distilled under reduced pressure to a volume of 12.6 L
  8. temperatureThe batch was then cooled to 15-25° C.
  9. custompurified water (19.9 L)
  10. additionadded
  11. stirringThe batch was stirred for 1 h 5 mins
  12. filtrationfiltered
  13. washthe filter cake washed with purified water (3×3.7 L)
  14. customthen dried under vacuum at 40° C.
  15. customto afford crude desired material (1978 g, 91.3%)
  16. customThe purification of the crude 8-[6-(3-dimethylaminopropoxy)pyridin-3-yl]-3-methyl-1-(oxan-4-yl)imidazo[5,4-c]quinolin-2-one (2066.9 g)
  17. additionCrude 8-[6-(3-dimethylaminopropoxy)pyridin-3-yl]-3-methyl-1-(oxan-4-yl)imidazo[5,4-c]quinolin-2-one (350.1 g) was charged to a 10 L flask with EtOH (7.7 L)
  18. temperatureheated until a solution
  19. customwas formed (68-73° C.)
  20. stirringthe solution stirred at 70-75° C. for 1 h
  21. filtrationThe hot solution was filtered
  22. washThe celite pad was washed with hot EtOH (2 L)
  23. customto remove any residual product
  24. additionon the celite and the initial filtrate charged to the vessel
  25. waitAfter completion of the 6 hot titrations carried out over 2 days
  26. distillationthe filtrate in the vessel was distilled under reduced pressure until the remaining filtrate (
  27. additioncould be added
  28. temperatureThe batch was then heated until a solution
  29. customwas formed (69° C.)
  30. distillationthe distillation
  31. customwas equal to 5 volumes of the input material (maximum distillation batch temperature=55° C.)
  32. distillationThe distillation
  33. temperaturethe batch cooled to 5-15° C.
  34. filtrationfiltered
  35. washwashed with EtOH (2.3 L)
  36. customdried

出典と根拠

ORDレコード
ord-b42970b6003c4130a257f12b659d9660
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09428503B2

反応ノート

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