1H-Pyrazol-3-amine, 5-methyl- → HCID 178486653、化合物

HRID 2100754ノート

反応式

HRID 2100754 の反応式
[C:1]([CH2:3][C:4]1[C:9]([C:10](O)=[O:11])=[CH:8][C:7]([C:13]([N:15]([CH3:17])[CH3:16])=[O:14])=[C:6]([O:18][CH3:19])[CH:5]=1)#[N:2].[NH2:20][C:21]1[CH:25]=[C:24]([CH3:26])[NH:23][N:22]=1>C(O)(=O)C>[CH3:16][N:15]([CH3:17])[C:13]([C:7]1[CH:8]=[C:9]2[C:4]([CH:3]=[C:1]([NH:20][C:21]3[CH:25]=[C:24]([CH3:26])[NH:23][N:22]=3)[N:2]=[C:10]2[OH:11])=[CH:5][C:6]=1[O:18][CH3:19])=[O:14]

参加物

4

反応物 2

HCID 931461H-Pyrazol-3-amine, 5-methyl-HCID 57799630HCID 57799630、化合物

生成物 1

HCID 178486653HCID 178486653、化合物収率 85%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
130 °C

実験手順

A mixture of 6-Cyanomethyl-4-methoxy-N,N-dimethyl-isophthalamic acid (2.0 g, 7.6 mmol), 3-amino-5-methylpyrazol (1.5 g, 15.44 mmol), acetic acid (10 ml) were sealed in microwave process vial (20 ml). The mixture was heated at 130° C. for 30 minutes under microwave irradiation. After removal of acetic acid, the residue was dissolved in 1.5 ml MeOH, and this solution was added dropwise to 30 ml water. After stirred for 1 hour, the solid was collected and was purified by flash column chromatography to give product (2.2 g, 85%). LC-MS: m/e 342 (MH+).

後処理

  1. customwere sealed in microwave process vial (20 ml)
  2. customAfter removal of acetic acid
  3. dissolutionthe residue was dissolved in 1.5 ml MeOH
  4. additionthis solution was added dropwise to 30 ml water
  5. customthe solid was collected
  6. customwas purified by flash column chromatography

出典と根拠

ORDレコード
ord-83135e71faa54c288857eb4bf2fc2bb0
出典データセット
uspto-grants-2009_08
特許番号
US07572809B2

反応ノート

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