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1,2-Dichloroethane → N-((4-benzyl-6-methyl-2-oxo-1,2-dihydropyridin-3-yl)methyl)-5-bromo-3-isopropyl-1-methyl-1H-indole-7-carboxamide

HRID 1616817
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HRID 1616817 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[C:9]([C:11]([OH:13])=O)[CH:10]=1)[N:7]([CH3:14])[CH:6]=[C:5]2[CH:15]([CH3:17])[CH3:16].Cl.[NH2:19][CH2:20][C:21]1[C:22](=[O:35])[NH:23][C:24]([CH3:34])=[CH:25][C:26]=1[CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.ON1C2N=CC=CC=2N=N1.C(Cl)CCl.CN1CCOCC1>O.CS(C)=O>[CH2:27]([C:26]1[CH:25]=[C:24]([CH3:34])[NH:23][C:22](=[O:35])[C:21]=1[CH2:20][NH:19][C:11]([C:9]1[CH:10]=[C:2]([Br:1])[CH:3]=[C:4]2[C:8]=1[N:7]([CH3:14])[CH:6]=[C:5]2[CH:15]([CH3:17])[CH3:16])=[O:13])[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 181649HOAtHCID 674669583-(aminomethyl)-4-benzyl-6-methylpyridin-2(1H)-one hydrochlorideHCID 678162465-bromo-1-methyl-3-(1-methylethyl)-1H-indole-7-carboxylic acid

생성물 1

HCID 67816369
N-((4-benzyl-6-methyl-2-oxo-1,2-dihydropyridin-3-yl)methyl)-5-bromo-3-isopropyl-1-methyl-1H-indole-7-carboxamide
수율 89%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

A 20 mL, oven dried vial was charged with 5-bromo-1-methyl-3-(1-methylethyl)-1H-indole-7-carboxylic acid (0.075 g, 0.253 mmol), 3-(aminomethyl)-4-benzyl-6-methylpyridin-2(1H)-one hydrochloride (0.080 g, 0.304 mmol), 1-hydroxy-7-azabenzotriazole (0.041 g, 0.304 mmol) and EDC (0.058 g, 0.304 mmol). Dimethyl sulfoxide (DMSO) (2 mL) was added via syringe, followed by N-methylmorpholine (0.111 mL, 1.013 mmol). The mixture was capped and stirred at RT over weekend. 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.) for 2 h. Collected the solids and further dried in a vacuum oven (45° C.) for 18 h to give N-((4-benzyl-6-methyl-2-oxo-1,2-dihydropyridin-3-yl)methyl)-5-bromo-3-isopropyl-1-methyl-1H-indole-7-carboxamide (120 mg, 0.225 mmol, 89% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 11.58 (s, 1H), 8.63 (t, J=4.9 Hz, 1H), 7.75 (d, J=1.8 Hz, 1H), 7.30 (m, 2H), 7.22 (m, 3H), 7.13 (s, 1H), 7.05 (d, J=1.8 Hz, 1H), 5.78 (s, 1H), 4.39 (d, J=4.8 Hz, 2H), 3.96 (s, 2H), 3.64 (s, 3H), 3.11 (dt, J=13.6, 6.8 Hz, 1H), 2.09 (s, 3H), 1.26 (m, 6H). MS (ES) [M+H]+ 506.3.

후처리

  1. customA 20 mL, oven dried vial
  2. customThe mixture was capped
  3. filtrationThe solids were filtered
  4. washwashed with water (10 mL), air
  5. customdried for 5 min
  6. waitplaced in a vacuum oven (40° C.) for 2 h
  7. customCollected the solids
  8. customfurther dried in a vacuum oven (45° C.) for 18 h

출처 및 근거

ORD 기록
ord-0741ccebe0cf4f499dc99034dca98ff6
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08765792B2

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