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1,4-Dioxane → HCID 67817708、化合物

HRID 1616802
ノート
印刷プレビュー

反応式

HRID 1616802 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([C:11]([NH:13][CH2:14][C:15]3[C:16](=[O:23])[NH:17][C:18]([CH3:22])=[CH:19][C:20]=3[CH3:21])=[O:12])[CH:10]=1)[N:7]([CH3:24])[CH:6]=[C:5]2[CH:25]([CH3:27])[CH3:26].Cl.[CH3:29][N:30]([CH2:32][C:33]1[CH:38]=[CH:37][C:36](B2OC(C)(C)C(C)(C)O2)=[CH:35][CH:34]=1)[CH3:31].P([O-])([O-])([O-])=O.[K+].[K+].[K+].O1CCOCC1>C(Cl)Cl.O>[CH3:29][N:30]([CH2:32][C:33]1[CH:38]=[CH:37][C:36]([C:2]2[CH:3]=[C:4]3[C:8](=[C:9]([C:11]([NH:13][CH2:14][C:15]4[C:16](=[O:23])[NH:17][C:18]([CH3:22])=[CH:19][C:20]=4[CH3:21])=[O:12])[CH:10]=2)[N:7]([CH3:24])[CH:6]=[C:5]3[CH:25]([CH3:26])[CH3:27])=[CH:35][CH:34]=1)[CH3:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 312751,4-DioxaneHCID 62657Potassium Phosphate, TribasicHCID 44118821Dimethyl({[4-(tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl]methyl})amine hydrochlorideHCID 57345388HCID 57345388、化合物

生成物 1

HCID 67817708HCID 67817708、化合物収率 37.5%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒

実験手順

In a glass pressure tube was added 5-bromo-N-[(4,6-dimethyl-2-oxo-1,2-dihydro-3-pyridinyl)methyl]-1-methyl-3-(1-methylethyl)-1H-indole-7-carboxamide (225 mg, 0.523 mmol), 4-(N,N-dimethylaminomethyl)phenylboronic acid pinacol ester hydrochloride (200 mg, 0.672 mmol), potassium phosphate (340 mg, 1.602 mmol), dioxane (12 mL) and water (3 mL). The reaction was stirred and purged with N2 then PdCl2 (dppf)-CH2Cl2 adduct (40 mg, 0.049 mmol) was added. The reaction was capped and stirred at 110° C. for 4 h LCMS indicated that the reaction was complete. The dark black reaction was transferred to a round bottom flask and evaporated to dryness. The crude material was purified by silica gel chromatography (Analogix, SF25-40 g, 0 to 70% CH2Cl2/20% (5% NH4OH in MeOH) in CH2Cl2). A short DASi column was used and the compound loaded as a suspension in CH2Cl2. The pure fractions were combined and evaporated to dryness to give the product as a very dark brown-black solid. The solid was taken up in CH2Cl2 and treated with Silicycle Si-Thiol derivatized silica gel (2 g, 1.46 mMol/g, cat. no. R51030B). After swirling for ˜30 minutes the mixture was filtered through a pad of Celite, washed with CH2Cl2, and evaporated to dryness. The now light yellow colored solid was dissolved in a small amount of CH2Cl2, triturated with hexanes, filtered and dried under vacuum to give 5-{4-[(dimethylamino)methyl]phenyl}-N-[(4,6-dimethyl-2-oxo-1,2-dihydro-3-pyridinyl)methyl]-1-methyl-3-(1-methylethyl)-1H-indole-7-carboxamide (95 mg, 0.196 mmol, 37.5% yield) as a light tan solid. 1H NMR (400 MHz, DMSO-d6) δ 11.50 (s, 1H), 8.50 (t, J=4.93 Hz, 1H), 7.83 (d, J=1.52 Hz, 1H), 7.68 (s, 1H), 7.66 (s, 1H), 7.40 (s, 1H), 7.38 (s, 1H), 7.33 (d, J=1.52 Hz, 1H), 7.10 (s, 1H), 5.87 (s, 1H), 4.36 (d, J=5.05 Hz, 2H), 3.69 (s, 3H), 3.34 (br. s., 3H), 3.22 (dt, J=6.73, 13.58 Hz, 1H), 2.26 (br. s., 6H), 2.24 (s, 2H), 2.11 (s, 3H), 1.31 (d, J=6.82 Hz, 6H). MS (ES)+m/e 485.3 [M+H]+.

後処理

  1. custompurged with N2
  2. customThe reaction was capped
  3. stirringstirred at 110° C. for 4 h LCMS
  4. customThe dark black reaction
  5. customwas transferred to a round bottom flask
  6. customevaporated to dryness
  7. customThe crude material was purified by silica gel chromatography (Analogix
  8. customevaporated to dryness
  9. customto give the product as a very dark brown-black solid
  10. filtrationthe mixture was filtered through a pad of Celite
  11. washwashed with CH2Cl2
  12. customevaporated to dryness
  13. dissolutionThe now light yellow colored solid was dissolved in a small amount of CH2Cl2
  14. customtriturated with hexanes
  15. filtrationfiltered
  16. customdried under vacuum

出典と根拠

ORDレコード
ord-d43c6e764202447c82df20a01e7ed948
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765792B2

反応ノート

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