تفاعل #1129733

ord-bd085724012041e6b953d5889ae4e57d

معادلة التفاعل

O=C([O-])[O-].[K+].[K+]
potassium carbonate
CC(C)(C)OC(=O)n1cc(C(=O)C#C[Si](C)(C)C)c2cnccc21
tert-butyl 3-(3-trimethylsilylpropynoyl)pyrrolo-[3,2-c]pyridine-1-carboxylate
N=C(N)Nc1ccccc1.O=C(O)O
phenylguanidine carbonate
O
water
c1ccc(Nc2nccc(-c3c[nH]c4ccncc34)n2)cc1
phenyl-[4-(1H-pyrrolo[3,2-c]pyridin-3-yl)pyrimidin-2-yl]amine
c1ccc(Nc2nccc(-c3c[nH]c4ccncc34)n2)cc1
phenyl[4-(1H-pyrrolo[3,2-c]pyridin-3-yl)pyrimidin-2-yl]-amine

ظروف التفاعل

درجة الحرارة
40°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture is heated at the boil for 68 hours
  2. 2
    درجة الحرارةAfter cooling
  3. 3
    أخرىThe precipitate formed
  4. 4
    ترشيحis filtered off with suction
  5. 5
    غسيلwashed with water
  6. 6
    أخرىdried in vacuo

الإجراء التجريبي

1.2 104 mg (0.75 mmol) of potassium carbonate are added to a solution of 103 mg (0.30 mmol of tert-butyl 3-(3-trimethylsilylpropynoyl)pyrrolo-[3,2-c]pyridine-1-carboxylate and 148 mg (0.75 mmol) of phenylguanidine carbonate in 1.5 ml of ethylene glycol monomethyl ether, and the mixture is heated at the boil for 68 hours. After cooling, 10 ml of water are added, and the mixture is stirred at 40° C. for 1 h. The precipitate formed is filtered off with suction, washed with water and dried in vacuo, giving phenyl-[4-(1H-pyrrolo[3,2-c]pyridin-3-yl)pyrimidin-2-yl]amine (“A1”) as pale-brown solid; ESI 287;

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08557977B2uspto-grants-2013_10