1-Butanol → HCID 12783669、化合物

HRID 372673ノート

反応式

HRID 372673 の反応式
[Na].Cl[C:3]1[NH:8][C:7](=[O:9])[C:6]([F:10])=[CH:5][N:4]=1.[CH2:11]([OH:15])[CH2:12][CH2:13][CH3:14]>>[CH2:11]([O:15][C:3]1[NH:8][C:7](=[O:9])[C:6]([F:10])=[CH:5][N:4]=1)[CH2:12][CH2:13][CH3:14]

参加物

4

反応物 3

HCID 2631-ButanolHCID 2553942-Chloro-5-fluoropyrimidin-4-olHCID 5360545Sodium

生成物 1

HCID 12783669HCID 12783669、化合物収率 91.9%

実験手順

A 5.8 g quantity of metal sodium is dissolved in 300 ml of absolute n-butanol, 14.9 g of 2-chloro-5-fluoropyrimidin-4-one is added to the solution and the mixture is heated in a sealed tube at 140° to 150° C for 5 hours for reaction. The solvent is distilled off from the reaction mixture, 50 ml of water is added to the residue and the pH of the mixture is adjusted to 4-5 to separate out crystals, which are recrystallized from ethanol to give 17.1 g of white crystalline 2-n-butoxy-5-fluoropyrimidin-4-one in a yield of 91.9%, m.p. 127°-129° C.

後処理

  1. temperaturethe mixture is heated in a sealed tube at 140° to 150° C for 5 hours for reaction
  2. distillationThe solvent is distilled off from the reaction mixture, 50 ml of water
  3. additionis added to the residue
  4. customto separate out crystals, which
  5. customare recrystallized from ethanol

出典と根拠

ORDレコード
ord-569e5438da574991b9c71c26f8073e1d
出典データセット
uspto-grants-1978_05
特許番号
US04092313

反応ノート

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