Acetic Acid → 6-Chloroquinazoline-2,4(1H,3H)-dione

HRID 1479403

反応式

HRID 1479403 の反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:3]=1[C:4](O)=[O:5].C(O)(=O)C.[O:16]([C:18]#[N:19])[Na].[OH-].[Na+]>O>[Cl:11][C:8]1[CH:7]=[C:3]2[C:2](=[CH:10][CH:9]=1)[NH:1][C:18](=[O:16])[NH:19][C:4]2=[O:5]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 124762-Amino-5-chlorobenzoic acidHCID 14798Sodium HydroxideHCID 178418852HCID 178418852、化合物

生成物 1

HCID 3039986-Chloroquinazoline-2,4(1H,3H)-dione

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
30 °C

実験手順

Into a 500-mL 3-necked round-bottom flask, was placed a solution of 2-amino-5-chlorobenzoic acid (10 g, 58.48 mmol, 1.00 equiv) in water (100 mL), acetic acid (8 g, 133.33 mmol, 2.24 equiv). This was followed by the addition of NaOCN (8.2 g, 126.15 mmol, 2.13 equiv). The mixture was stirred for 30 mins at 30° C. To this was added sodium hydroxide (86 g, 2.15 mol, 37.00 equiv). The resulting solution was stirred overnight at 30° C. The solids were collected by filtration. The residue was dissolved in water. The pH value of the solution was adjusted to 7 with hydrogen chloride (12 mol/L). The solids were collected by filtration. This resulted in 5 g (44%) of 6-chloroquinazoline-2,4(1H,3H)-dione as a white solid.

後処理

  1. customInto a 500-mL 3-necked round-bottom flask, was placed
  2. stirringThe resulting solution was stirred overnight at 30° C
  3. filtrationThe solids were collected by filtration
  4. dissolutionThe residue was dissolved in water
  5. filtrationThe solids were collected by filtration
  6. customThis resulted in 5 g (44%) of 6-chloroquinazoline-2,4(1H,3H)-dione as a white solid

出典と根拠

ORDレコード
ord-d58aec76a6944f73a1ec4d609b007ea7
出典データセット
uspto-grants-2016_08
特許番号
US09408840B2

関連ノート

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