Ammonia → 4-amino-1-benzyl-3-nitro-1H-pyridin-2-one

HRID 1376210ノート

反応式

HRID 1376210 の反応式
[CH2:1]([N:8]1[CH:13]=[CH:12][C:11](Cl)=[C:10]([N+:15]([O-:17])=[O:16])[C:9]1=[O:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH3:19]>C1COCC1>[NH2:19][C:11]1[CH:12]=[CH:13][N:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:9](=[O:18])[C:10]=1[N+:15]([O-:17])=[O:16]

参加物

4

反応物 2

HCID 222AmmoniaHCID 249444631-Benzyl-4-chloro-3-nitropyridin-2(1H)-one

生成物 1

HCID 219476414-amino-1-benzyl-3-nitro-1H-pyridin-2-one収率 91.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1-benzyl-4-chloro-3-nitro-1H-pyridin-2-one (1.30 g, 4.91 mmol) and 28% aqueous ammonia (4.92 g, 39.3 mmol) in THF (30 mL) was stirred at room temp for 17 h. The solvent was evaporated under reduced pressure and water was added to the residue. The resulting precipitate was collected by filtration, and washed with water to give 4-amino-1-benzyl-3-nitro-1H-pyridin-2-one (1.10 g, 91% yield). 1H-NMR (DMSO): δ 8.13 (m, 2H), 7.69 (d, 1H, J=8.0 Hz), 7.31 (m, 5H), 5.94 (d, 1H, J=8.0 Hz), 4.96 (s, 2H). MS: calculated for C12H11N3O3+H 246.1; found: 246.2.

後処理

  1. customThe solvent was evaporated under reduced pressure and water
  2. additionwas added to the residue
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed with water

出典と根拠

ORDレコード
ord-144df5b152584093a5ff6bfe76dd43d4
出典データセット
uspto-grants-2007_01
特許番号
US07169926B1

反応ノート

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