تفاعل #1435740

ord-d113e0255ddd4a95b781dda3acb68082

معادلة التفاعل

CN1CCN(c2cc(I)c(N)cn2)CC1
4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-ylamine
CCN(C(C)C)C(C)C
N,N-diisopropyl ethyl amine
CC(C)(C(=O)Cl)c1cc(C(F)(F)F)cc(C(F)(F)F)c1
2-(3,5-bis-trifluoromethyl-phenyl)-2-methyl-propionyl chloride
CN1CCN(c2cc(I)c(NC(=O)C(C)(C)c3cc(C(F)(F)F)cc(C(F)(F)F)c3)cn2)CC1
crude title compound
المردود 112.3%
CN1CCN(c2cc(I)c(NC(=O)C(C)(C)c3cc(C(F)(F)F)cc(C(F)(F)F)c3)cn2)CC1
2-(3,5-Bis-trifluoromethyl-phenyl)-N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-isobutyramide
المردود 112.3%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux
  2. 2
    درجة الحرارةAfter cooling to room temperature the reaction mixture
  3. 3
    غسيلwas washed with 20 ml of a 1 M aqueous sodium carbonate solution and 20 ml water
  4. 4
    تجفيفThe combined organic layers were dried over sodium sulfate
  5. 5
    تركيزconcentrated in vacuo

الإجراء التجريبي

To a suspension of 1.60 g (5.03 mmol) 4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-ylamine and 975 mg (7.54 mmol) N,N-diisopropyl ethyl amine in 16 ml dichloromethane was added dropwise 1.76 g (5.53 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-2-methyl-propionyl chloride at 0° C. The reaction mixture was stirred for 2 h at room temperature and 2 h at reflux. After cooling to room temperature the reaction mixture was washed with 20 ml of a 1 M aqueous sodium carbonate solution and 20 ml water. The combined organic layers were dried over sodium sulfate and concentrated in vacuo to give 3.39 g (100%) of the crude title compound as a brown oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07211579B2uspto-grants-2007_05