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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
ノート
印刷プレビュー

反応式

HRID 1616817 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 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

生成物 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
収率 89%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water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 (0.075 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.

後処理

  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

出典と根拠

ORDレコード
ord-0741ccebe0cf4f499dc99034dca98ff6
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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