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1,2-Dichloroethane → 5-bromo-1-methyl-3-(1-methylethyl)-N-[(4-methyl-2-oxo-1,2-dihydro-3-pyridinyl)methyl]-1H-indole-7-carboxamide

HRID 1616818
ノート
印刷プレビュー

反応式

HRID 1616818 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([C:11]([OH:13])=[O:12])[CH:10]=1)[N:7]([CH3:14])[CH:6]=[C:5]2[CH:15]([CH3:17])[CH3:16].[NH2:18][CH2:19][C:20]1[C:21](=[O:27])[NH:22][CH:23]=[CH:24][C:25]=1[CH3:26].ON1C2N=CC=CC=2N=N1.C(Cl)CCl.CN1CCOCC1>C(Cl)(Cl)Cl.ClCCl.O.CS(C)=O>[NH3:7].[CH3:11][OH:12].[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([C:11]([NH:18][CH2:19][C:20]3[C:21](=[O:27])[NH:22][CH:23]=[CH:24][C:25]=3[CH3:26])=[O:13])[CH:10]=1)[N:7]([CH3:14])[CH:6]=[C:5]2[CH:15]([CH3:17])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 181649HOAtHCID 678159882(1H)-Pyridinone, 3-(aminomethyl)-4-methyl-HCID 678162465-bromo-1-methyl-3-(1-methylethyl)-1H-indole-7-carboxylic acid

生成物 2

HCID 21705897Ammonia methanol収率 10%
HCID 67811954
5-bromo-1-methyl-3-(1-methylethyl)-N-[(4-methyl-2-oxo-1,2-dihydro-3-pyridinyl)methyl]-1H-indole-7-carboxamide
収率 118.3%

試薬・触媒・溶媒 4

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

A 20 mL, oven dried vial was charged with 5-bromo-1-methyl-3-(1-methylethyl)-1H-indole-7-carboxylic acid (0.10 g, 0.338 mmol), 3-(aminomethyl)-4-methyl-2(1H)-pyridinone (0.088 g, 0.506 mmol), 1-hydroxy-7-azabenzotriazole (0.069 g, 0.506 mmol) and EDC (0.097 g, 0.506 mmol). To the mixture was added dimethyl sulfoxide (DMSO) (3 mL) via syringe, followed by N-methylmorpholine (0.148 mL, 1.351 mmol). The mixture was capped and stirred at RT overnight. The reaction was poured into 60 mL water and the resultant mixture stirred for 10 min, then placed in a freezer for 10 min. The solids were filtered, washed with water (10 mL), air dried for 5 min, and placed in a vacuum oven (40° C.). The solid was dissolved in DCM/MeOH and absorbed onto silica gel and concentrated in vacuo to dryness. Purification by column chromatography (12 g Isco GOLD silica column; Gradient B: 5-85%, A: dichloromethane, B: 10% 2 M ammonia/methanol in chloroform) gave 5-bromo-1-methyl-3-(1-methylethyl)-N-[(4-methyl-2-oxo-1,2-dihydro-3-pyridinyl)methyl]-1H-indole-7-carboxamide (85 mg, 0.200 mmol, 59.3% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.25 (d, J=6.82 Hz, 6H) 2.26 (s, 3H) 3.03-3.17 (m, 1H) 3.64 (s, 3H) 4.34 (d, J=4.80 Hz, 2H) 6.05 (d, J=6.57 Hz, 1H) 7.09 (d, J=1.77 Hz, 1H) 7.14 (s, 1H) 7.22 (d, J=6.82 Hz, 1H) 7.75 (d, J=1.77 Hz, 1H) 8.57 (t, J=4.80 Hz, 1H) 11.48 (br. s., 1H). MS (ES) [M+H]+ 415.9.

後処理

  1. customA 20 mL, oven dried vial
  2. customThe mixture was capped
  3. waitplaced in a freezer for 10 min
  4. filtrationThe solids were filtered
  5. washwashed with water (10 mL), air
  6. customdried for 5 min
  7. customplaced in a vacuum oven (40° C.)
  8. dissolutionThe solid was dissolved in DCM/MeOH
  9. customabsorbed onto silica gel
  10. concentrationconcentrated in vacuo to dryness
  11. customPurification by column chromatography (12 g Isco GOLD silica column

出典と根拠

ORDレコード
ord-8d2fc664f8ff4dd29d8f1f6407fd37ce
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

読み込み中…

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