Amitrole → HCID 178515486、化合物

HRID 923342

反応式

HRID 923342 の反応式
[N:1]1[NH:2][C:3]([NH2:6])=[N:4][CH:5]=1.[O:7]1[CH2:12][CH2:11][O:10][C:9]2[CH:13]=[C:14]([C:17](=O)[CH2:18][C:19](OCC)=[O:20])[CH:15]=[CH:16][C:8]1=2>C(O)(=O)C>[O:7]1[CH2:12][CH2:11][O:10][C:9]2[CH:13]=[C:14]([C:17]3[NH:6][C:3]4[N:2]([N:1]=[CH:5][N:4]=4)[C:19](=[O:20])[CH:18]=3)[CH:15]=[CH:16][C:8]1=2

参加物

4

反応物 2

HCID 1639AmitroleHCID 15315318Ethyl 2,3-dihydro-β-oxo-1,4-benzodioxin-6-propanoate

生成物 1

HCID 178515486HCID 178515486、化合物収率 15%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
120 °C

実験手順

A mixture of 2H-1,2,4-triazol-3-amine (200 mg, 2.38 mmol, 1.00 equiv), acetic acid (3 mL), and ethyl 3-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-3-oxopropanoate (600 mg, 2.40 mmol, 1.01 equiv) was stirred for 24 hr at 120° C. and then concentrated to dryness. The resulting solid was washed with MeOH and collected by filtration. The solid was dissolved in 15 mL of NH4OH (aq.) and filtered. The filtrate was adjusted to pH 5 with HOAc. The resulting solid was collected by filtration and washed with water. The solid was dried to get 95 mg (15%) of 5-(2,3-dihydrobenzo[b][1,4]dioxin-6-yl)-[1,2,4]triazolo[1,5-α]pyrimidin-7(4H)-one as a white solid.

後処理

  1. concentrationconcentrated to dryness
  2. washThe resulting solid was washed with MeOH
  3. filtrationcollected by filtration
  4. dissolutionThe solid was dissolved in 15 mL of NH4OH (aq.)
  5. filtrationfiltered
  6. filtrationThe resulting solid was collected by filtration
  7. washwashed with water
  8. customThe solid was dried

出典と根拠

ORDレコード
ord-bde312b457114b68bc8a3ac5eae6bfc4
出典データセット
uspto-grants-2016_03
特許番号
US09278973B2

関連ノート

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