Acetic Anhydride → HCID 22160577, compound

HRID 1089280Notes

Reaction equation

HRID 1089280 reaction equation
C(O[C:5](=[O:7])C)(=O)C.[NH2:8][C:9]1[C:10]([Cl:16])=[N:11][C:12]([Cl:15])=[N:13][CH:14]=1>C(O)=O>[Cl:15][C:12]1[N:11]=[C:10]([Cl:16])[C:9]([NH:8][CH:5]=[O:7])=[CH:14][N:13]=1

Participants

4

Reactant 2

HCID 7918Acetic AnhydrideHCID 2577975-Amino-2,4-dichloropyrimidine

Product 1

HCID 22160577HCID 22160577, compound

Reagents, catalysts & solvents 1

HCID 284Formic AcidSolvent

Conditions

Temperature
20 °C

Procedure

Acetic anhydride (12 ml) was added to a mixture of 5-amino-2,4-dichloropyrimidine (2.34 g, 14.4 mmol) and formic acid (30 ml) at 0° C. The mixture was stirred at 20° C. for 4 hours, evaporated to dryness and co-evaporated with toluene. The crystalline product was homogeneous on t.l.c. (chloroform-methanol, 15.1) and used without further purification. (2.74 g, 100%). IR: υmax (KBr) 3445, 3350, 3240, 1635, 1570, 1515, 1415 cm-1. 1H NMR δH [(CD3)2SO] 8.45 (1H,s,H.2), 9.40 (1H,s,CH), 10.40 (1H,br.s, NH).

Workup

  1. customevaporated to dryness and co-evaporated with toluene
  2. custom(chloroform-methanol, 15.1) and used without further purification

Sources & evidence

ORD record
ord-15c22d4847274695850bb5ca1a64dfde
Source dataset
uspto-grants-1990_10
Patent number
US04965270

Reaction notes

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