HCID 13376462、化合物 → HCID 13376463、化合物

HRID 986649ノート

反応式

HRID 986649 の反応式
[F:1][CH2:2][C:3]1[N:12]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][C:14]=2[CH3:20])[C:11](=[O:21])[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([N+:22]([O-])=O)[CH:9]=2)[N:4]=1>CO.Cl>[F:1][CH2:2][C:3]1[N:12]([C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][C:14]=2[CH3:20])[C:11](=[O:21])[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([NH2:22])[CH:9]=2)[N:4]=1

参加物

4

反応物 1

HCID 13376462HCID 13376462、化合物

生成物 1

HCID 13376463HCID 13376463、化合物収率 66.1%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒

実験手順

2.0 g of 2-fluoromethyl-3-(2,4-dimethylphenyl)-6-nitro-4(3H)-quinazolinone are suspended in 35 ml of methanol, and a solution of 5.4 g of stannous chloride dihydrate in 5 ml of conc. hydrochloric acid is added dropwise thereto under ice-cooling and stirring. Then, the mixture is stirred at room temperature overnight. The mixture is concentrated under reduced pressure to remove methanol, and water is added to the residue. The aqueous mixture is neutralized with sodium bicarbonate, and chloroform is added thereto. After stirring the mixture, insoluble materials are filtered off. The chloroform solution is separated from the filtrate and concentrated under reduced pressure to give a crystalline residue. The thus-obtained crystals (1.4 g) are recrystallized from isopropanol. 1.2 g of 2-fluoromethyl-3-(2,4-dimethylphenyl)-6-amino-4(3H)-quinazolinone are obtained as pale yellow prisms.

後処理

  1. temperatureunder ice-cooling
  2. stirringThen, the mixture is stirred at room temperature overnight
  3. concentrationThe mixture is concentrated under reduced pressure
  4. customto remove methanol, and water
  5. additionis added to the residue
  6. additionis added
  7. stirringAfter stirring the mixture, insoluble materials
  8. filtrationare filtered off
  9. customThe chloroform solution is separated from the filtrate
  10. concentrationconcentrated under reduced pressure
  11. customto give a crystalline residue
  12. customThe thus-obtained crystals (1.4 g) are recrystallized from isopropanol

出典と根拠

ORDレコード
ord-566e4a41ac0449f1b6c34a50087623c3
出典データセット
uspto-grants-1987_12
特許番号
US04714702

反応ノート

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