Hydrochloric Acid → 3-Chloro-3-methyl-2-nitroso-1-(5-methyl-2-nitro-1H-imidazol-1-yl)butane

HRID 278388

反応式

HRID 278388 の反応式
[CH3:1][C:2]1[N:6]([CH2:7][CH:8]=[C:9]([CH3:11])[CH3:10])[C:5]([N+:12]([O-:14])=[O:13])=[N:4][CH:3]=1.[N+:15]([O-:23])(OCCC(C)C)=O.[ClH:24]>>[Cl:24][C:9]([CH3:11])([CH3:10])[CH:8]([N:15]=[O:23])[CH2:7][N:6]1[C:2]([CH3:1])=[CH:3][N:4]=[C:5]1[N+:12]([O-:14])=[O:13]

参加物

4

実験手順

3-Chloro-3-methyl-2-nitroso-1-(5-methyl-2-nitro-1H-imidazol-1-yl) butane was prepared in 60% yield from 1-(5-methyl-2-nitro-1H-imidazol-1-yl)-3-methyl-2-butene (1.0 g, 5.12 mmol, Example 27), isoamyl nitrate (5.0 mL) and concentrated HCl (5.0 mL) following the procedure described for the preparation of its positional isomer (Example 27B) as a light blue solid; mp. 102-105° C. (decomp); 1H NMR (DMSO-d6) δ 1.73 [s, 6H, C(CH3)2], 2.32(s, 3H, imi-CH3), 5.53(s, 2H, NCH2), 6.97 ( s. 1H, imi-CH) and 11.58 (s, 1H, NOH). MS m/e 261 (M+H)+.

後処理

  1. customdescribed for the preparation of its positional isomer (Example 27B) as a light blue solid

出典と根拠

ORDレコード
ord-d4c52a84c0cd49e38b76c22e563f7c75
出典データセット
uspto-grants-2002_03
特許番号
US06359120B1

関連ノート

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