反応 #167896

ord-9116dc6336ab4c4e9bb40f58c13e565f

反応方程式

Cc1c(N2CCNCC2)nn2c(I)c(-c3ccc(F)cc3)nc2c1C
2-(4-fluorophenyl)-3-iodo-7,8-dimethyl-6-piperazin-1-ylimidazo[1,2-b]pyridazine
CN(C)c1ccccn1
dimethylaminopyridine
CC(C)(C)OC(=O)OC(C)(C)C
di-tert-butyl carbonate
Cc1c(N2CCN(C(=O)OC(C)(C)C)CC2)nn2c(I)c(-c3ccc(F)cc3)nc2c1C
product
収率 78.4%
Cc1c(N2CCN(C(=O)OC(C)(C)C)CC2)nn2c(I)c(-c3ccc(F)cc3)nc2c1C
tert-Butyl 4-[2-(4-fluorophenyl)-3-iodo-7,8-dimethylimidazo[1,2-b]pyridazin-6-yl]piperazine-1-carboxylate
収率 78.4%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solvent is then evaporated off
  2. 2
    その他the solid obtained
  3. 3
    その他is recrystallized from acetonitrile

実験手順

A solution of 0.70 g (1.55 mmol) of 2-(4-fluorophenyl)-3-iodo-7,8-dimethyl-6-piperazin-1-ylimidazo[1,2-b]pyridazine and 19 mg (0.16 mmol) of dimethylaminopyridine in 10 mL of tetrahydrofuran is treated with 0.41 g (1.9 mmol) of di-tert-butyl carbonate for 1 hour. The solvent is then evaporated off and the solid obtained is recrystallized from acetonitrile. 0.67 g of product is thus isolated after drying.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08846676B2uspto-grants-2014_09