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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
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HRID 1616818 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 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

생성물 2

HCID 21705897Ammonia methanol수율 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
수율 118.3%

시약·촉매·용매 4

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8d2fc664f8ff4dd29d8f1f6407fd37ce
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765792B2

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