1,2-Dichloroethane → HCID 67467953, 화합물

HRID 42449

반응식

HRID 42449 반응식
[CH3:1][CH:2]([N:4]1[C:12]2[C:11]([O:13][CH3:14])=[CH:10][CH:9]=[C:8]([C:15]([OH:17])=O)[C:7]=2[CH:6]=[CH:5]1)[CH3:3].[NH2:18][CH2:19][C:20]1[C:21](=[O:30])[NH:22][C:23]([CH3:29])=[CH:24][C:25]=1[CH2:26][CH2:27][CH3:28].ON1C2N=CC=CC=2N=N1.C(Cl)CCl.CN1CCOCC1>O.CS(C)=O>[CH3:3][CH:2]([N:4]1[C:12]2[C:11]([O:13][CH3:14])=[CH:10][CH:9]=[C:8]([C:15]([NH:18][CH2:19][C:20]3[C:21](=[O:30])[NH:22][C:23]([CH3:29])=[CH:24][C:25]=3[CH2:26][CH2:27][CH3:28])=[O:17])[C:7]=2[CH:6]=[CH:5]1)[CH3:1]

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 79724-MethylmorpholineHCID 181649HOAtHCID 671241403-(Aminomethyl)-6-methyl-4-propylpyridin-2(1H)-oneacetateHCID 674686821-(1-Methylethyl)-7-(methyloxy)-1H-indole-4-carboxylic acid

생성물 1

HCID 67467953HCID 67467953, 화합물수율 60.8%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

Added 1-(1-methylethyl)-7-(methyloxy)-1H-indole-4-carboxylic acid (160 mg, 0.686 mmol), 3-(aminomethyl)-6-methyl-4-propyl-2(1H)-pyridinone (186 mg, 0.857 mmol), 1-hydroxy-7-azabenzotriazole (187 mg, 1.372 mmol), EDC (263 mg, 1.372 mmol) and N-methylmorpholine (0.302 mL, 2.74 mmol) to DMSO (10 mL) and stirred mixture at RT for 16 h. Added 25 ml of water and stirred for 10 minutes. Filtered off solids and dried in vacuo. The solids were purified by column chromatography (Biotage; 0% to 15% gradient MeOH:DCM; 10 g-HP-silica gel column) to give 165 mg of 1-(1-methylethyl)-N-[(6-methyl-2-oxo-4-propyl-1,2-dihydro-3-pyridinyl)methyl]-7-(methyloxy)-1H-indole-4-carboxamide.

후처리

  1. stirringstirred for 10 minutes
  2. filtrationFiltered off solids
  3. customdried in vacuo
  4. customThe solids were purified by column chromatography (Biotage; 0% to 15% gradient MeOH:DCM; 10 g-HP-silica gel column)

출처 및 근거

ORD 기록
ord-2afcf149aed4450c94b1257efecfe8ae
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536179B2

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