6-Methyl-2-nitropyridin-3-ol → 2-Amino-6-methylpyridin-3-ol

HRID 24056

反応式

HRID 24056 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([N+:8]([O-])=O)[C:5]([OH:11])=[CH:4][CH:3]=1>[Pd].C(OCC)(=O)C>[NH2:8][C:6]1[C:5]([OH:11])=[CH:4][CH:3]=[C:2]([CH3:1])[N:7]=1

参加物

4

反応物 1

HCID 848016-Methyl-2-nitropyridin-3-ol

生成物 1

HCID 885002-Amino-6-methylpyridin-3-ol収率 98,678.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 6-methyl-2-nitro-pyridin-3-ol (18.5 g, 0.120 mmol), 10% palladium on activated carbon (1.35 g), and ethyl acetate (240 mL) was hydrogenated for 3 days. The mixture was filtered through Celite and washed with methanol/ethylacetate (5%). The filtrate and washing were combined and concentrated to give the title compound (14.7 g, 99% yield) as a pale brown solid. 1H NMR (DMSO-d6) δ 9.19 (bs, 1H), 6.73 (d, 1H, J=7.6 Hz), 6.12 (d, 1H, J=7.6 Hz), 5.36 (bs, 2H), 2.15 (s, 3H).

後処理

  1. filtrationThe mixture was filtered through Celite
  2. washwashed with methanol/ethylacetate (5%)
  3. washThe filtrate and washing
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-9ced7b6581684eca95fe4d1a3fb3dbc2
出典データセット
uspto-grants-2005_02
特許番号
US06855722B2

関連ノート

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