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Potassium Phosphate, Tribasic → Methyl 7-(2-morpholinoethoxy)-2-(3-(trifluoromethyl)phenyl)-5h-pyrido[3,2-b]indole-4-carboxylate

HRID 2410768
ノート
印刷プレビュー

反応式

HRID 2410768 の反応式
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:4]=[C:5](B(O)O)[CH:6]=[CH:7][CH:8]=1.Br[C:15]1[CH:16]=[C:17]([C:37]([O:39][CH3:40])=[O:38])[C:18]2[NH:19][C:20]3[CH:21]=[C:22]([O:28][CH2:29][CH2:30][N:31]4[CH2:36][CH2:35][O:34][CH2:33][CH2:32]4)[CH:23]=[CH:24][C:25]=3[C:26]=2[N:27]=1.[O-]P([O-])([O-])=O.[K+].[K+].[K+].C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=CC=2OC)CCCCC1>CC([O-])=O.CC([O-])=O.[Pd+2]>[O:34]1[CH2:35][CH2:36][N:31]([CH2:30][CH2:29][O:28][C:22]2[CH:23]=[CH:24][C:25]3[C:26]4[N:27]=[C:15]([C:5]5[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:13])([F:12])[F:1])[CH:4]=5)[CH:16]=[C:17]([C:37]([O:39][CH3:40])=[O:38])[C:18]=4[NH:19][C:20]=3[CH:21]=2)[CH2:32][CH2:33]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 62657Potassium Phosphate, TribasicHCID 27343883-(Trifluoromethyl)phenylboronic acidHCID 112698722-Dicyclohexylphosphino-2',6'-dimethoxybiphenyl2 回HCID 86663030methyl 2-bromo-7-(2-morpholinoethoxy)-5H-pyrido[3,2-b]indole-4-carboxylate

生成物 1

HCID 66604728Methyl 7-(2-morpholinoethoxy)-2-(3-(trifluoromethyl)phenyl)-5h-pyrido[3,2-b]indole-4-carboxylate
収率 102%

試薬・触媒・溶媒 1

HCID 167845palladium(II) acetate触媒2 回

反応条件

温度
70 °C

実験手順

A mixture of 3-(trifluoromethyl)phenylboronic acid (51 mg, 0.27 mmol), methyl 2-bromo-7-(2-morpholinoethoxy)-5H-pyrido[3,2-b]indole-4-carboxylate (90 mg, 0.21 mmol), powdered potassium phosphate tribasic (114 mg, 0.539 mmol), dicyclohexyl(2′,6′-dimethoxybiphenyl-2-yl)phosphine (17 mg, 0.041 mmol), and Pd(OAc)2 (4.7 mg, 0.021 mmol) in a microwave vial was flushed with nitrogen. THF (1 mL) was added, the vial was capped, and the reaction was heated in a 70° C. oil bath for 18 hr. Additional Pd(OAc)2 (4.7 mg, 0.021 mmol) and dicyclohexyl(2′,6′-dimethoxybiphenyl-2-yl)phosphine (17 mg, 0.041 mmol) were added, the vial was resealed, and heating was continued for 16 hr. The reaction was filtered and the collected solid was washed with THF. The filtrate was applied onto an SCX column and washed with DCM and then MeOH. Release with 2 N NH3 in MeOH afforded crude methyl 7-(2-morpholinoethoxy)-2-(3-(trifluoromethyl)phenyl)-5H-pyrido[3,2-b]indole-4-carboxylate (107 mg). This was suspended in 7 N NH3 in MeOH (5 mL) in a sealed microwave vial and heated at 80° C. overnight. Preparative HPLC (100×30 mm Luna C18 column, gradient elution with A:B=30:70 to A:B=0:100 [A=10 mM NH4OAc in 5% aqueous CH3CN; B=10 mM NH4OAc in 95% aqueous CH3CN] over 20 min) followed by removal of the solvents on a SPEEDVAC® gave 7-(2-morpholinoethoxy)-2-(3-(trifluoromethyl)phenyl)-5H-pyrido[3,2-b]indole-4-carboxamide (48 mg, 0.094 mmol, 44% yield) as a yellow solid. MS (ESI) m/z 483.1 (M−H). 1H NMR (500 MHz, DMSO-d6) δ ppm 11.51 (1H, s), 8.62 (3H, s), 8.47 (1H, s), 8.16 (1H, d, J=8.55 Hz), 7.92 (1H, s), 7.69-7.83 (2H, m), 7.31 (1H, d, J=1.53 Hz), 6.92 (1H, dd, J=8.70, 1.68 Hz), 4.19 (2H, t, J=5.49 Hz), 3.61 (4H, t, J=4.43 Hz), 2.77 (2H, t, J=5.49 Hz), 2.51 (4H, br. s.).

後処理

  1. customwas flushed with nitrogen
  2. additionTHF (1 mL) was added
  3. customthe vial was capped
  4. temperatureheating
  5. filtrationThe reaction was filtered
  6. washthe collected solid was washed with THF
  7. washwashed with DCM

出典と根拠

ORDレコード
ord-cb4e090e6a944038b56b6b1834cf9b3e
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08815840B2

反応ノート

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