Water → HCID 86601060、化合物

HRID 31069ノート

反応式

HRID 31069 の反応式
[NH2:1][C:2]1[N:7]([CH2:8][CH2:9][O:10][CH3:11])[C:6](=[S:12])[NH:5][C:4](=[O:13])[CH:3]=1.[N:14]([O-])=[O:15].[Na+].O>C(O)(=O)C>[NH2:1][C:2]1[N:7]([CH2:8][CH2:9][O:10][CH3:11])[C:6](=[S:12])[NH:5][C:4](=[O:13])[C:3]=1[N:14]=[O:15]

参加物

5

反応物 3

HCID 962WaterHCID 31844116-amino-1-(2-methoxyethyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-oneHCID 23668193Sodium Nitrite

生成物 1

HCID 86601060HCID 86601060、化合物収率 37%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
75 °C

実験手順

6-Amino-1-(2-methoxy-ethyl)-2-thioxo-2,3-dihydro-1H-pyrimidin-4-one (1.0 g, 5.0 mmol) was suspended in 10% acetic acid (20 mL). Sodium nitrite (0.38 g, 5.5 mmol) was added and the resulting mixture was heated at 75° C. for 1 h. The reaction mixture became first pink and then purple. Water (20 mL) was added and the reaction mixture was put in the fridge overnight. The purple solid was collected by filtration and washed with water to give the title compound (0.42 g, 37%). A second crop of product (0.22 g, 19%) was obtained by reducing the volume of the purple filtrate. The crude product was used in the following step without further purification.

後処理

  1. customwas put in the fridge overnight
  2. filtrationThe purple solid was collected by filtration
  3. washwashed with water

出典と根拠

ORDレコード
ord-26259cb3d8ef4266ae17b6c1f6777f60
出典データセット
uspto-grants-2008_09
特許番号
US07425560B2

反応ノート

読み込み中…