Water → HCID 86601060, 화합물

HRID 31069노트

반응식

HRID 31069 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 86601060HCID 86601060, 화합물수율 37%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
75 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-26259cb3d8ef4266ae17b6c1f6777f60
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425560B2

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