Dimethylformamide → Acetate hexane

HRID 325094ノート

反応式

HRID 325094 の反応式
Cl.NC1N2N=C(C3[O:13][CH:14]=[CH:15]C=3)N=C2C=C(N2CCNCC2)N=1.[C:23]1(CCBr)[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.C(N(CC)CC)C.CN(C=[O:43])C>>[C:14]([O-:43])(=[O:13])[CH3:15].[CH3:27][CH2:28][CH2:23][CH2:24][CH2:25][CH3:26]

参加物

5

反応物 4

HCID 6228DimethylformamideHCID 7666Phenethyl bromideHCID 8471TriethylamineHCID 220024325-Amino-2-(2-furyl)-7-piperazinyl[1,2,4]triazolo[1,5-c]-pyrimidine hydrochloride

生成物 1

HCID 22139250Acetate hexane

反応条件

温度
60 °C

実験手順

In 10 ml of DMF, 400 mg (1.04 mmol) of Compound 43 obtained in Example 43 was dissolved, and 0.51 ml (3.6 mmol) of 2-phenylethyl bromide and 1 ml of triethylamine were added thereto, followed by stirring at 60° C. for 2 hours. The reaction mixture was extracted by adding chloroform and water, and the organic phase was dried over anhydrous magnesium sulfate. After evaporation of the solvent under reduced pressure, the residue was purified by silica gel column chromatography [chloroform-methanol (97:3)] and recrystallized from ethyl. acetate-hexane to give 369 mg (yield: 95%) of Compound 46 as light gray powder.

後処理

  1. extractionThe reaction mixture was extracted
  2. additionby adding chloroform and water
  3. dry with materialthe organic phase was dried over anhydrous magnesium sulfate
  4. customAfter evaporation of the solvent under reduced pressure
  5. customthe residue was purified by silica gel column chromatography [chloroform-methanol (97:3)]
  6. customrecrystallized from ethyl

出典と根拠

ORDレコード
ord-f8d96c12c1364e309b040b8fbf6bae6f
出典データセット
uspto-grants-2001_04
特許番号
US06222035B1

反応ノート

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