Ammonia → 5,6-Diamino-1-pentyl-2-thioxo-2,3-dihydropyrimidin-4(1H)-one

HRID 2368546노트

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HRID 2368546 반응식
[NH2:1][C:2]1[N:7]([CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:6](=[S:13])[NH:5][C:4](=[O:14])[C:3]=1[N:15]=O.N.O.S(S([O-])=O)([O-])=O.[Na+].[Na+]>C(O)(=O)C>[NH2:15][C:3]1[C:4](=[O:14])[NH:5][C:6](=[S:13])[N:7]([CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:2]=1[NH2:1]

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 962WaterHCID 24489Sodium DithioniteHCID 576001906-Amino-5-nitroso-1-pentyl-2-thioxo-2,3-dihydropyrimidin-4(1H)-one

생성물 1

HCID 576002545,6-Diamino-1-pentyl-2-thioxo-2,3-dihydropyrimidin-4(1H)-one수율 86.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
75 °C

실험 절차

To a mixture of 6-amino-1-pentyl-5-nitroso-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (6.4 g, 0.0264 mol), aqueous ammonia (60 mL, 0.60 mol) and water (60 mL) at 75° C. was added sodium dithionite (9.0 g, 0.050 mol) in small portions. After the addition was complete, the color of the solution changed from red to pale yellow. After stirring at 75° C. for another 5 mins, a precipitate was formed. Stirring was continued at room temperature for 1.5 h. The solution was then neutralized with 10% acetic acid (150 mL). The solid was filtered and washed with water to yield the product (4.5 g, 86.1%). LCMS calculated for C9H17N4OS: (M+H) 229.1. Found 229.1.

후처리

  1. additionAfter the addition
  2. customa precipitate was formed
  3. stirringStirring
  4. waitwas continued at room temperature for 1.5 h
  5. filtrationThe solid was filtered
  6. washwashed with water

출처 및 근거

ORD 기록
ord-eca63c6d9a5b4ca18530c3109105cf28
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08703783B2

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