Acetic Acid → HCID 136386277、化合物

HRID 68720ノート

反応式

HRID 68720 の反応式
[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:5]=[C:4]([CH2:13][CH3:14])[C:3]=1[C:15]([NH2:17])=[O:16].N[C:19](N)=[O:20].CC(O)=O>[OH-].[Na+]>[CH2:13]([C:4]1[C:3]2[C:15](=[O:16])[NH:17][C:19](=[O:20])[NH:1][C:2]=2[N:6]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[N:5]=1)[CH3:14]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 1176UreaHCID 540196475-amino-3-ethyl-1-phenyl-1H-pyrazole-4-carboxamide

生成物 1

HCID 136386277HCID 136386277、化合物

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

反応条件

温度
200 °C

実験手順

Into a 100-mL 3-necked round-bottom flask, was placed 5-amino-3-ethyl-1-phenyl-1H-pyrazole-4-carboxamide (1 g, 4.35 mmol, 1.00 equiv) at room temperature. To the resulting mixture was then added urea (1.75 g, 29.17 mmol, 6.70 equiv), in portions at room temperature. The resulting solution was stirred for 1 h at 200° C. The resulting mixture was then cooled to room temperature. The residue was dissolved in sodium hydroxide (250 mL). The pH value of the solution was adjusted to about 5 with AcOH (conc.). The solids were collected by filtration to yield 3-ethyl-1-phenyl-1H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione as a white solid. MS (m/z): 257 [MH+].

後処理

  1. customInto a 100-mL 3-necked round-bottom flask, was placed
  2. customat room temperature
  3. customat room temperature
  4. temperatureThe resulting mixture was then cooled to room temperature
  5. filtrationThe solids were collected by filtration

出典と根拠

ORDレコード
ord-4e374c925c824bdca5f708ad3e529ec2
出典データセット
uspto-grants-2014_09
特許番号
US08822447B2

反応ノート

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