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Citric Acid → 4-((3-(4-(1H-1,2,4-Triazol-1-yl)benzyl)-4-chloro-2-methoxyquinolin-6-yl)(hydroxy)(1-methyl-1H-imidazol-5-yl)methyl)benzonitrile

HRID 926580
ノート
印刷プレビュー

反応式

HRID 926580 の反応式
Br[C:2]1[N:6]([CH3:7])[CH:5]=[N:4][CH:3]=1.[N:8]1([C:13]2[CH:42]=[CH:41][C:16]([CH2:17][C:18]3[C:19]([O:39][CH3:40])=[N:20][C:21]4[C:26]([C:27]=3[Cl:28])=[CH:25][C:24]([C:29]([C:31]3[CH:38]=[CH:37][C:34]([C:35]#[N:36])=[CH:33][CH:32]=3)=[O:30])=[CH:23][CH:22]=4)=[CH:15][CH:14]=2)[CH:12]=[N:11][CH:10]=[N:9]1.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>O1CCCC1>[N:8]1([C:13]2[CH:14]=[CH:15][C:16]([CH2:17][C:18]3[C:19]([O:39][CH3:40])=[N:20][C:21]4[C:26]([C:27]=3[Cl:28])=[CH:25][C:24]([C:29]([OH:30])([C:2]3[N:6]([CH3:7])[CH:5]=[N:4][CH:3]=3)[C:31]3[CH:38]=[CH:37][C:34]([C:35]#[N:36])=[CH:33][CH:32]=3)=[CH:23][CH:22]=4)=[CH:41][CH:42]=2)[CH:12]=[N:11][CH:10]=[N:9]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 311Citric AcidHCID 15152585-Bromo-1-methyl-1H-imidazoleHCID 1180062474-(3-(4-(1H-1,2,4-Triazol-1-yl)benzyl)-4-chloro-2-methoxyquinoline-6-carbonyl)benzonitrile2 回

生成物 1

HCID 1180065414-((3-(4-(1H-1,2,4-Triazol-1-yl)benzyl)-4-chloro-2-methoxyquinolin-6-yl)(hydroxy)(1-methyl-1H-imidazol-5-yl)methyl)benzonitrile

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
3 回

実験手順

A solution of isopropylmagnesium chloride-lithium chloride complex in tetrahydrofuran (1.3 M, 0.986 mL, 1.28 mmol) was added dropwise to an ice-water cooled, stirring suspension of 5-bromo-1-methyl-1H-imidazole (241 mg, 1.50 mmol) in dry tetrahydrofuran (6 mL). After 5 minutes, the flask was removed from the cooling bath and the white suspension was stirred at 23° C. After 10 minutes, the Grignard suspension was added to an ice-water cooled, stirring mixture containing 4-(3-(4-(1H-1,2,4-triazol-1-yl)benzyl)-4-chloro-2-methoxyquinoline-6-carbonyl)benzonitrile (205 mg, 0.427 mmol, Intermediate 16: step e) and lanthanum(III) chloride bis(lithium chloride) complex (0.6 M solution in tetrahydrofuran, 1.42 mL, 0.854 mmol) in dry tetrahydrofuran (8 mL). After 20 minutes, 1 M aqueous citric acid solution (1 mL) was added. The flask was removed from the cooling bath and then ethyl acetate (100 mL) was added. Additional 1 M aqueous citric acid solution (˜15 mL) was added until the mixture was comprised of two homogeneous layers, at which point saturated aqueous sodium bicarbonate solution was added until the pH of the aqueous layer was ˜8 by litmus paper test. The layers were separated. The aqueous layer was extracted with ethyl acetate (20 mL). The organic layers were combined and the combined solution was dried over sodium sulfate. The dried solution was filtered. Silica gel (5 g) was added to the filtrate and the mixture was concentrated by rotary evaporation to afford a free-flowing powder. The powder was loaded onto a silica gel column for flash-column chromatography purification. Elution with dichloromethane initially, grading to 10% methanol-dichloromethane provided the title compound as a white solid. 1H NMR (500 MHz, CDCl3) δ ppm 8.45 (s, 1H), 8.10 (d, J=2.2 Hz, 1H), 8.06 (s, 1H), 7.81 (d, J=8.8 Hz, 1H), 7.65 (d, J=8.5 Hz, 2H), 7.58-7.51 (m, 5H), 7.44-7.38 (m, 3H), 6.41 (d, J=1.1 Hz, 1H), 4.33 (s, 2H), 4.09 (s, 3H), 3.94 (s, 1H), 3.38 (s, 3H); MS (ESI): mass calcd. C31H24ClN7O2, 561.2. m/z found, 562.1 [M+H]+.

後処理

  1. temperaturecooled
  2. customthe flask was removed from the cooling bath
  3. stirringthe white suspension was stirred at 23° C
  4. waitAfter 10 minutes
  5. additionthe Grignard suspension was added to an ice-water
  6. temperaturecooled
  7. stirringstirring mixture
  8. waitAfter 20 minutes
  9. customThe flask was removed from the cooling bath
  10. additionethyl acetate (100 mL) was added
  11. additionAdditional 1 M aqueous citric acid solution (˜15 mL) was added until the mixture
  12. additionwas added until the pH of the aqueous layer
  13. customThe layers were separated
  14. extractionThe aqueous layer was extracted with ethyl acetate (20 mL)
  15. dry with materialthe combined solution was dried over sodium sulfate
  16. filtrationThe dried solution was filtered
  17. additionSilica gel (5 g) was added to the filtrate
  18. concentrationthe mixture was concentrated by rotary evaporation
  19. customto afford a free-flowing powder
  20. customThe powder was loaded onto a silica gel column for flash-column chromatography purification
  21. washElution with dichloromethane initially

出典と根拠

ORDレコード
ord-c2cb1e074ef546c09b501cb326e8753c
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09284308B2

反応ノート

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