Methylamine → N,1-dimethyl-1H-indazole-3-carboxamide

HRID 1581678

反応式

HRID 1581678 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([C:11]([O:13]C)=O)=[N:3]1.[CH3:15][NH2:16]>CO>[CH3:15][NH:16][C:11]([C:4]1[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[N:2]([CH3:1])[N:3]=1)=[O:13]

参加物

4

反応物 2

HCID 6329MethylamineHCID 13900574Methyl 1-methyl-1H-indazole-3-carboxylate

生成物 1

HCID 22593809N,1-dimethyl-1H-indazole-3-carboxamide収率 89%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A suspension of methyl 1-methyl-1H-indazole-3-carboxylate (3.88 g, 20.4 mmole) in 40% aqueous CH3NH2 (100 mL) and MeOH (5 mL) was stirred at RT for 4 hr, during which time a homogeneous solution formed. The solution was concentrated to approximately ⅓ volume and the precipitated solid was collected by filtration, washed with H2O, and dried in vacuo to give the title compound (3.42 g. 89%) as a pale yellow solid: 1H NMR (300 MHz, CDCl3) δ 8.24 (m, 1H), 7.47 (m, 2H), 7.34 (m, 1H), 6.95 (br s, 1H), 4.19 (s, 3H), 3.05 (d, J=12.0 Hz, 3H).

後処理

  1. customformed
  2. concentrationThe solution was concentrated to approximately ⅓ volume
  3. filtrationthe precipitated solid was collected by filtration
  4. washwashed with H2O
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-ddaaaec190684643a93261a58376e3d6
出典データセット
uspto-grants-2004_05
特許番号
US06730684B1

関連ノート

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