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Ethanol → 7-Methyl-8-propyl-[1,2,4]triazolo[1,5-C]pyrimidine

HRID 916660
ノート
印刷プレビュー

反応式

HRID 916660 の反応式
[CH2:1]([C:4]1[C:5](Cl)=[N:6][CH:7]=[N:8][C:9]=1[CH3:10])[CH2:2][CH3:3].O.[NH2:13][NH2:14].[CH3:15]CO>>[CH3:10][C:9]1[N:8]=[CH:7][N:13]2[N:14]=[CH:15][N:6]=[C:5]2[C:4]=1[CH2:1][CH2:2][CH3:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)HCID 223131564-Chloro-6-methyl-5-propylpyrimidine

生成物 1

HCID 534715537-Methyl-8-propyl-[1,2,4]triazolo[1,5-C]pyrimidine

反応条件

温度
100 °C

実験手順

A mixture of 4-chloro-6-methyl-5-propyl-pyrimidine (101) (500 mg, 2.93 mmol) and hydrazine monohydrate (880 mg, 17.6 mmol) in EtOH (15 mL) is heated in a sealed tube at 100° C. overnight. On cooling, the solvent is removed and to the residue is added water (15 mL). The solid is filtered and washed with water (5 mL) and ether (10 mL). The solid is then heated in acetic acid (10 mL) in a sealed tube at 110° C. overnight. The excess acetic acid is removed under vacuum. The residue is neutralized with aqueous sodium bicarbonate and then extracted with ethyl acetate. On drying, the solvent is removed to give the product (168).

後処理

  1. temperatureOn cooling
  2. customthe solvent is removed and to the residue
  3. additionis added water (15 mL)
  4. filtrationThe solid is filtered
  5. washwashed with water (5 mL) and ether (10 mL)
  6. temperatureThe solid is then heated in acetic acid (10 mL) in a sealed tube at 110° C. overnight
  7. customThe excess acetic acid is removed under vacuum
  8. extractionextracted with ethyl acetate
  9. customOn drying
  10. customthe solvent is removed

出典と根拠

ORDレコード
ord-de45d286aad448c68137effb4b2a52f1
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07271170B2

反応ノート

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