تفاعل #70533

معادلة التفاعل

3-Methylbenzoic acid

HATU

DIPEA

6-(1H-indol-4-yl)-1H-indazol-4-amine

→

title compound

N-[6-(1H-Indol-4-yl)-1H-indazol-4-yl]-3-methylbenzamide

المذيبات

DMF

DMF

ظروف التفاعل

المعالجة

1. 1
   workup.WAITto stand at room temperature for 16 hrs
2. 2
   أخرىSolvent was removed in vacuo
3. 3
   workup.DISSOLUTIONthe product re-dissolved in chloroform (0.3 mL)
4. 4
   غسيلProduct was eluted after 2 hr with ethyl acetate/methanol (1:1, 3.2 mL)
5. 5
   تركيزconcentrated under a stream of nitrogen using blow down apparatus
6. 6
   أخرىPurification by MDAP (Method C)

الإجراء التجريبي

3-Methylbenzoic acid (60 mg, 0.44 mmol) was treated with HATU (168 mg, 0.44 mmol) in DMF (0.750 mL) and DIPEA (0.15 mL, 0.86 mmol). The mixture was shaken for five minutes prior to treatment with 6-(1H-indol-4-yl)-1H-indazol-4-amine (50 mg, 0.2 mmol) in DMF (0.350 mL) and was then left to stand at room temperature for 16 hrs. Solvent was removed in vacuo and the product re-dissolved in chloroform (0.3 mL) prior to application on to a pre-conditioned (methanol then chloroform) NH2 cartridge (1 g). Product was eluted after 2 hr with ethyl acetate/methanol (1:1, 3.2 mL), and concentrated under a stream of nitrogen using blow down apparatus. Purification by MDAP (Method C) afforded the title compound.

المصدر