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Methyl iodide → diethyl 4-(3-methyl-4(3H)-quinazolinon-2-yl)benzylphosphonate

HRID 482444
ノート
印刷プレビュー

反応式

HRID 482444 の反応式
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([C:12]2[CH:26]=[CH:25][C:15]([CH2:16][P:17](=[O:24])([O:21][CH2:22][CH3:23])[O:18][CH2:19][CH3:20])=[CH:14][CH:13]=2)[N:3]=1.[CH3:27]C(C)([O-])C.[K+].CI>CO>[CH3:27][N:3]1[C:2](=[O:1])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]1[C:12]1[CH:13]=[CH:14][C:15]([CH2:16][P:17](=[O:24])([O:21][CH2:22][CH3:23])[O:18][CH2:19][CH3:20])=[CH:25][CH:26]=1
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

5

反応物 3

HCID 6328Methyl iodideHCID 23665647Potassium tert-butoxideHCID 178476844HCID 178476844、化合物

生成物 1

HCID 10643860diethyl 4-(3-methyl-4(3H)-quinazolinon-2-yl)benzylphosphonate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
40 °C

実験手順

A 5.9 g quantity of diethyl 4-(4-hydroxyquinazolin-2-yl)benzylphosphonate, 1.8 g of potassium tert-butoxide and 2.3 g of methyl iodide were suspended in 100 ml of anhydrous methanol and stirred with heating at 40° C. for 16 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: methylene chloride: methanol=100:1) and the crude crystals thus obtained were recrystallized from methylene chloride-n-hexane to provide 3.0 g of the title compound as colorless crystals.

後処理

  1. customAfter completion of the reaction
  2. distillationthe solvent was distilled off under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (eluent: methylene chloride: methanol=100:1)
  4. customthe crude crystals thus obtained
  5. customwere recrystallized from methylene chloride-n-hexane

出典と根拠

ORDレコード
ord-1e960697b65048cf946b43a3a37e22a9
出典データセット
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05798344

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート