Methyl iodide → [3-(4-Methoxy-phenyl)-[1,2,4]triazolo[3,4-a]phthalazin-6-yl]-[3-(2-methyl-2H-tetrazol-5-yl)-phenyl]-amine

HRID 424404ノート

反応式

HRID 424404 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:13]3[N:14]=[C:15]([NH:22][C:23]4[CH:28]=[CH:27][CH:26]=[C:25]([C:29]5[N:30]=[N:31][NH:32][N:33]=5)[CH:24]=4)[C:16]4[C:21]([C:12]3=[N:11][N:10]=2)=[CH:20][CH:19]=[CH:18][CH:17]=4)=[CH:5][CH:4]=1.CI.[C:36]([O-])([O-])=O.[K+].[K+]>CN(C=O)C.CC(C)=O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[N:13]3[N:14]=[C:15]([NH:22][C:23]4[CH:28]=[CH:27][CH:26]=[C:25]([C:29]5[N:30]=[N:31][N:32]([CH3:36])[N:33]=5)[CH:24]=4)[C:16]4[C:21]([C:12]3=[N:11][N:10]=2)=[CH:20][CH:19]=[CH:18][CH:17]=4)=[CH:7][CH:8]=1

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 11575700[3-(4-Methoxy-phenyl)-[1,2,4]triazolo[3,4-a]phthalazin-6-yl]-[3-(2H-tetrazol-5-yl)-phenyl]-amine

生成物 1

HCID 11705056[3-(4-Methoxy-phenyl)-[1,2,4]triazolo[3,4-a]phthalazin-6-yl]-[3-(2-methyl-2H-tetrazol-5-yl)-phenyl]-amine収率 20.5%

試薬・触媒・溶媒 1

HCID 18184436N,N-dimethylformamide acetone溶媒

実験手順

To a suspension of [3-(4-methoxy-phenyl)-[1,2,4]triazolo[3,4-a]phthalazin-6-yl]-[3-(2H-tetrazol-5-yl)-phenyl]-amine (compound T3) (111 mg, 0.25 mmol) in a mixture of DMF/acetone 1:1 (8 mL) are added methyl iodide (79 μg, 1.25 mmol) and K2CO3 (53 mg, 0.37 mmol). The mixture is stirred at room temperature over night. The reaction mixture is concentrated and water is added. The resulting precipitate is filtered and washed with methanol to yield 23 mg of the title compound as white powder.

後処理

  1. concentrationThe reaction mixture is concentrated
  2. additionwater is added
  3. filtrationThe resulting precipitate is filtered
  4. washwashed with methanol

出典と根拠

ORDレコード
ord-fbe4b5baf876440382f949b15e17aa62
出典データセット
uspto-grants-2012_01
特許番号
US08106047B2

反応ノート

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