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1H-Pyrazol-3-amine, 5-methyl- → HCID 178493402、化合物

HRID 2100748
ノート
印刷プレビュー

反応式

HRID 2100748 の反応式
[C:1]([CH2:3][C:4]1[CH:12]=[C:11]([O:13][CH3:14])[CH:10]=[C:9]([O:15][CH3:16])[C:5]=1[C:6](O)=[O:7])#[N:2].[NH2:17][C:18]1[CH:22]=[C:21]([CH3:23])[NH:20][N:19]=1>C(O)(=O)C>[CH3:14][O:13][C:11]1[CH:12]=[C:4]2[C:5](=[C:9]([O:15][CH3:16])[CH:10]=1)[C:6]([OH:7])=[N:2][C:1]([NH:17][C:18]1[CH:22]=[C:21]([CH3:23])[NH:20][N:19]=1)=[CH:3]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 931461H-Pyrazol-3-amine, 5-methyl-HCID 57799575HCID 57799575、化合物

生成物 1

HCID 178493402HCID 178493402、化合物収率 255.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
140 °C

実験手順

A mixture of 2-Cyanomethyl-4,6-dimethoxy-benzoic acid (1.75 g×3), 3-amino-5-methylpyrazole (1.5 g×3) in acetic acid (10 ml×3) were sealed in microwave process vial (20 ml×3). The mixture was heated at 140° C. for 30 minutes under microwave irradiation. The mixture was evaporated to oil, and the oil was dissolved in 1.5 ml MeOH. This solution was added dropwise to 50 ml water. After stirred for 1 hour, solid was collected and was purified by flash column chromatography to give product (6.07 g, 85%). LC-MS: m/e 301 (MH+).

後処理

  1. customwere sealed in microwave process vial (20 ml×3)
  2. customThe mixture was evaporated to oil
  3. dissolutionthe oil was dissolved in 1.5 ml MeOH
  4. additionThis solution was added dropwise to 50 ml water
  5. customsolid was collected
  6. customwas purified by flash column chromatography

出典と根拠

ORDレコード
ord-17a6e9b771c04baa8a7f931965911dd0
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07572809B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート