Phosphorus oxychloride → HCID 178420858, Verbindung

HRID 710513

Reaktionsgleichung

Reaktionsgleichung von HRID 710513
[N:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]([NH:12][NH2:13])=[O:11])=[CH:9][C:4]=2[NH:3][CH:2]=1.CO[C:16]1[C:21]([O:22][CH3:23])=[CH:20][CH:19]=[CH:18][C:17]=1[CH2:24][CH2:25][C:26](Cl)=O.[O:29]=P(Cl)(Cl)Cl>>[O:29]1[C:20]2[CH:19]=[CH:18][C:17]([CH2:24][CH2:25][C:26]3[O:11][C:10]([C:8]4[CH:7]=[CH:6][C:5]5[NH:1][CH:2]=[N:3][C:4]=5[CH:9]=4)=[N:12][N:13]=3)=[CH:16][C:21]=2[O:22][CH2:23]1

Komponenten

4

Versuchsvorschrift

The compound was synthesized starting from benzimidazol-5-carbohydrazide (176 mg, 1 mmol), TEA (0.153 ml; 1.1 mmol), 2,3-dimethoxyphenylpropionylchloride (228 mg, 1.1 mmol) and POCl3 (0.5 ml; 5.5 mmol) as described in method 1; yield: 0.016 mg (4.6%); MS m/z: 351.3 [M+H]+; 1H-NMR (DMSO d6, 400 MHz): δ 3.06-3.10 (m, 2H); 3.17-3.21 (m, 2H); 3.73 (s, 3H); 3.79 (s, 3H); 6.82-6.84 (m, 1H); 6.90-6.92 (m, 1H); 6.95-6.99 (m, 1H); 7.75-7.77 (m, 1H); 7.80-7.82 (m, 1H); 8.14 (br s, 1H); 8.41 (s, 1H); HPLC (METHOD [A]): rt 11.49 min (94.5%)

Aufarbeitung

  1. customThe compound was synthesized
  2. customrt 11.49 min (94.5%)

Quellen und Nachweise

ORD-Eintrag
ord-ee4000bb78084baea09d3e46c7444b9e
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09181233B2

Verknüpfte Notizen

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