Trifluoroacetic acid → N-(4-Chloro-3-(4,5-dihydro-3-(4-iodophenyl)-5-oxo-1,2,4-triazol-1-yl)benzyl)isobutyramide

HRID 59402

反応式

HRID 59402 の反応式
[I:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([N:8]=[C:9]=[O:10])=O)=[CH:4][CH:3]=1.[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([CH2:20][NH:21][C:22](=[O:26])[CH:23]([CH3:25])[CH3:24])=[CH:16][C:15]=1[NH:27][NH:28]C(OC(C)(C)C)=O.FC(F)(F)C(O)=O>C(Cl)Cl>[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([CH2:20][NH:21][C:22](=[O:26])[CH:23]([CH3:25])[CH3:24])=[CH:16][C:15]=1[N:27]1[C:9](=[O:10])[NH:8][C:6]([C:5]2[CH:11]=[CH:12][C:2]([I:1])=[CH:3][CH:4]=2)=[N:28]1

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 149137404-Iodobenzoyl isocyanateHCID 90065680tert-Butyl 2-(2-chloro-5-{[(2-methylpropanoyl)amino]methyl}phenyl)hydrazinecarboxylate

生成物 1

HCID 136492445N-(4-Chloro-3-(4,5-dihydro-3-(4-iodophenyl)-5-oxo-1,2,4-triazol-1-yl)benzyl)isobutyramide収率 34.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The title compound was prepared according to the procedure described in Example-83 by using 4-iodobenzoyl isocyanate (Intermediate-67, 1.500 g), tert-butyl 2-(2-chloro-5-{[(2-methylpropanoyl)amino]methyl}phenyl)hydrazinecarboxylate (Intermediate-97, 1.0 g), DCM (20 mL), and trifluoro acetic acid (5.0 mL) to afford 0.500 g of the desired product. 1H NMR (400 MHz, DMSO d6): δ 1.02 (d, J=6.9 Hz, 6H), 2.44 (m, 1H), 4.28 (d, J=8.7 Hz, 2H), 7.28 (br s, 1H), 7.35 (d, J=7.8 Hz, 1H), 7.44 (s, 1H), 7.61 (d, J=8.7 Hz, 1H), 7.91 (d, J=8.1 Hz, 2H), 8.38 (m, 1H), 12.61 (m, 1H); MS (m/z): 495.7 (M−H)−.

後処理

  1. customThe title compound was prepared

出典と根拠

ORDレコード
ord-a5390c7637484582a4a456af50bce18e
出典データセット
uspto-grants-2016_09
特許番号
US09439890B2

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