benzyl (3-(2-(dimethylamino)ethoxy)-1-methyl-1H-pyrazol-5-yl)carbamate → 3-[2-(dimethylamino)ethoxy]-1-methyl-1H-pyrazol-5-amine

HRID 577737

反応式

HRID 577737 の反応式
[CH3:1][N:2]([CH3:23])[CH2:3][CH2:4][O:5][C:6]1[CH:10]=[C:9]([NH:11]C(=O)OCC2C=CC=CC=2)[N:8]([CH3:22])[N:7]=1>CO.[Pd]>[CH3:1][N:2]([CH3:23])[CH2:3][CH2:4][O:5][C:6]1[CH:10]=[C:9]([NH2:11])[N:8]([CH3:22])[N:7]=1

参加物

4

反応物 1

HCID 86679669benzyl (3-(2-(dimethylamino)ethoxy)-1-methyl-1H-pyrazol-5-yl)carbamate

生成物 1

HCID 866796703-[2-(dimethylamino)ethoxy]-1-methyl-1H-pyrazol-5-amine収率 79.1%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A mixture of benzyl (3-(2-(dimethylamino)ethoxy)-1-methyl-1H-pyrazol-5-yl)carbamate (1.42 g, 4.46 mmol) and 10% Pd/C (0.2 g) in MeOH (40 mL) was hydrogenated with fully inflated H2 balloon at rt overnight. The mixture was filtered and the filtrate was concentrated in vacuo to give the title compound (0.65 g, 79% yield) as a pale solid. 1H NMR (400 MHz, CDCl3) δ ppm 5.04 (s, 1H), 4.19-4.16 (t, 2H), 3.51 (s, 3H), 3.45 (bs, 2H), 2.67-2.64 (t, 2H), 2.32 (s, 6H). m/z for C8H16N4O 185.14 (M+H)+.

後処理

  1. filtrationThe mixture was filtered
  2. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-e6062623629c4ccbb420a70d63da79f3
出典データセット
uspto-grants-2015_05
特許番号
US09040547B2

関連ノート

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