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Water → 7-fluoro-3-methyl-2-((1-methylcyclobutyl)amino)-8-((6R)-6-methyl-4-oxo-1,4,5,6-tetrahydropyrrolo[3,4-b]pyrrol-2-yl)-4(3H)-quinazolinone

HRID 1056396
ノート
印刷プレビュー

反応式

HRID 1056396 の反応式
Br[C:2]1[C:3]([F:20])=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([NH:12][C:13]1([CH3:17])[CH2:16][CH2:15][CH2:14]1)[N:8]([CH3:18])[C:7]2=[O:19].[CH3:21][C@@H:22]1[C:26]2[NH:27][C:28](B3OC(C)(C)C(C)(C)O3)=[CH:29][C:25]=2[C:24](=[O:39])[NH:23]1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].O>O1CCOCC1>[F:20][C:3]1[C:2]([C:28]2[NH:27][C:26]3[C@@H:22]([CH3:21])[NH:23][C:24](=[O:39])[C:25]=3[CH:29]=2)=[C:11]2[C:6]([C:7](=[O:19])[N:8]([CH3:18])[C:9]([NH:12][C:13]3([CH3:17])[CH2:16][CH2:15][CH2:14]3)=[N:10]2)=[CH:5][CH:4]=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 962WaterHCID 62657Potassium Phosphate, TribasicHCID 89781988(R)-6-methyl-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5,6-dihydropyrrolo[3,4-b]pyrrol-4(1H)-oneHCID 897820938-bromo-7-fluoro-3-methyl-2-((1-methylcyclobutyl)amino)-quinazolin-4(3H)-one

生成物 1

HCID 897832747-fluoro-3-methyl-2-((1-methylcyclobutyl)amino)-8-((6R)-6-methyl-4-oxo-1,4,5,6-tetrahydropyrrolo[3,4-b]pyrrol-2-yl)-4(3H)-quinazolinone
収率 17.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

A mixture of 8-bromo-7-fluoro-3-methyl-2-((1-methylcyclobutyl)amino)quinazolin-4(3H)-one (502a, 120 mg, 0.353 mmol), (R)-6-methyl-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5,6-dihydropyrrolo[3,4-b]pyrrol-4(1H)-one (705, 237 mg, 0.705 mmol), bis(di-tert-butyl(4-dimethylaminophenyl)phosphine)-dichloropalladium (II) (12.49 mg, 0.018 mmol), and potassium phosphate (225 mg, 1.058 mmol) in 1,4-dioxane (2.82 mL)/water (0.70 mL) was sparged with nitrogen for 3 min at RT; the red reaction mixture was then heated to 80° C. for 45 min. The reaction mixture was diluted with EtOAc (100 mL), added to a separatory funnel, and washed with saturated aqueous NaHCO3 (2×100 mL); the organic layer was separated, dried over Na2SO4, and concentrated. The crude product was loaded onto the column and was purified via automated flash chromatography (silica gel) with 0-5% 2 M ammonia in MeOH/DCM to give (R)-7-fluoro-3-methyl-8-(6-methyl-4-oxo-1,4,5,6-tetrahydropyrrolo[3,4-b]pyrrol-2-yl)-2((1-methylcyclobutyl)amino)quinazolin-4(3H)-one (502, 24 mg, 0.061 mmol, 17% yield) as an off-white solid. 1H NMR (400 MHz, CDCl3) δ ppm 1.58 (s, 3H) 1.78 (s, 3H) 1.98-2.15 (m, 2H) 2.27-2.42 (m, 3H) 2.42-2.52 (m, 1H) 3.56 (s, 3H) 4.69 (q, J=6.65 Hz, 1H) 5.08 (s, 1H) 6.01 (s, 1H) 7.00 (dd, J=11.54, 8.80 Hz, 1H) 7.08 (d, J=4.11 Hz, 1H) 8.01 (dd, J=8.80, 6.06 Hz, 1H) 12.76 (br. s., 1H). 19F NMR (376 MHz, CDCl3) δ ppm −99.57 (s, 1F). MS (ESI, pos. ion) m/z: 369.0 (M+1).

後処理

  1. customwas sparged with nitrogen for 3 min at RT
  2. additionThe reaction mixture was diluted with EtOAc (100 mL)
  3. additionadded to a separatory funnel
  4. washwashed with saturated aqueous NaHCO3 (2×100 mL)
  5. customthe organic layer was separated
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated
  8. customwas purified

出典と根拠

ORDレコード
ord-fd32f23a98084b2da75da3e0964f6152
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394297B2

反応ノート

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