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 424404노트

반응식

HRID 424404 반응식
[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

참가 물질

5

반응물 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

생성물 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]-amine수율 20.5%

시약·촉매·용매 1

HCID 18184436N,N-dimethylformamide acetone용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-fbe4b5baf876440382f949b15e17aa62
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106047B2

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