Methyl iodide → 6,7-Dimethoxy-2-[4-(1-methyl-2-benzimidazolyl)-1-piperazinyl]-4-quinazolinamine

HRID 1703181ノート

反応式

HRID 1703181 の反応式
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]1[CH2:15][CH2:14][N:13]([C:16]2[N:25]=[C:24]([NH2:26])[C:23]3[C:18](=[CH:19][C:20]([O:29][CH3:30])=[C:21]([O:27][CH3:28])[CH:22]=3)[N:17]=2)[CH2:12][CH2:11]1.[CH3:31]I>CS(C)=O>[CH3:28][O:27][C:21]1[CH:22]=[C:23]2[C:18](=[CH:19][C:20]=1[O:29][CH3:30])[N:17]=[C:16]([N:13]1[CH2:14][CH2:15][N:10]([C:2]3[N:3]([CH3:31])[C:4]4[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=4[N:1]=3)[CH2:11][CH2:12]1)[N:25]=[C:24]2[NH2:26]

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 130363862-[4-(1H-2-Benzimidazolyl)-1-piperazinyl]-6,7-dimethoxy-4-quinazolinamine

生成物 1

HCID 130616916,7-Dimethoxy-2-[4-(1-methyl-2-benzimidazolyl)-1-piperazinyl]-4-quinazolinamine

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixture of 2-[4-(1H-2-benzimidazolyl)-1-piperazinyl]-6,7-dimethoxy-4-quinazolinamine (0.75 g, described in Example 10) and methyl iodide (1.0 ml) in dimethyl sulfoxide (10 ml) was stirred at room temperature for 4 hr and poured into ice. The resulting mixture was extracted with chloroform. The organic extract was washed with water, dried over sodium sulfate and evaporated. The residue was chromatographed through silica gel using 4% methanol in chloroform. The appropriate fractions were combined and evaporated to give a residue (0.42 g) of the title compound. The latter residue was crystallized from hexane-chloroform: mp 249°-251° C.; ir (CHCl3) 3400 and 3300 cm-1 ; uv max (MeOH) 213 (ε=49,870), 250 (ε=64,830); 284 (ε=26,545) and 341 nm (ε=6,565); and Anal. Calcd. for C22H25N7O2 : C, 62.99% H, 6.01% N, 23.37% and Found: C, 62,81% H, 6.18% N, 23.71%.

後処理

  1. additionpoured into ice
  2. extractionThe resulting mixture was extracted with chloroform
  3. extractionThe organic extract
  4. washwas washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe residue was chromatographed through silica gel using 4% methanol in chloroform
  8. customevaporated

出典と根拠

ORDレコード
ord-fe40937c03df4565822837ca945111d4
出典データセット
uspto-grants-1982_09
特許番号
US04351832

反応ノート

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