Formaldehyde → 5-cyano-1-(N-hydroxymethyl-2,4,6-trichloroanilino)-2,4-pyrimidinedione

HRID 648160

反応式

HRID 648160 の反応式
[C:1]([C:3]1[C:4](=[O:20])[NH:5][C:6](=[O:19])[N:7]([NH:9][C:10]2[C:15]([Cl:16])=[CH:14][C:13]([Cl:17])=[CH:12][C:11]=2[Cl:18])[CH:8]=1)#[N:2].[CH2:21]=[O:22].O>C(O)=O>[C:1]([C:3]1[C:4](=[O:20])[NH:5][C:6](=[O:19])[N:7]([N:9]([CH2:21][OH:22])[C:10]2[C:11]([Cl:18])=[CH:12][C:13]([Cl:17])=[CH:14][C:15]=2[Cl:16])[CH:8]=1)#[N:2]

参加物

5

反応物 3

HCID 712Formaldehyde2 回HCID 962WaterHCID 132322481-(2,4,6-Trichloroanilino)-5-cyano-2,4-pyrimidinedione

生成物 1

HCID 132322565-cyano-1-(N-hydroxymethyl-2,4,6-trichloroanilino)-2,4-pyrimidinedione

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒2 回

実験手順

Two grams of 5-cyano-1-(2,4,6-trichloroanilino)-2,4-pyrimidinedione is added to 1.6 ml of 35% formaldehyde in enough 95% formic acid to effect stirring. The mixture is heated to reflux and 95% formic acid is added dropwise until the solid is dissolved. The mixture is refluxed overnight, after which 3.2 ml of aqueous formaldehyde is added and refluxing is continued for another 8 hours. The reaction mixture is poured into water and the precipitate is filtered to yield the compound 5-cyano-1-(N-hydroxymethyl-2,4,6-trichloroanilino)-2,4-pyrimidinedione, m.p.>300°.

後処理

  1. temperatureThe mixture is heated
  2. temperatureto reflux
  3. dissolutionis dissolved
  4. temperatureThe mixture is refluxed overnight
  5. temperaturerefluxing
  6. filtrationthe precipitate is filtered

出典と根拠

ORDレコード
ord-37d9669e2a2c4ebb893df8d04c38f158
出典データセット
uspto-grants-1983_10
特許番号
US04411839

関連ノート

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