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

HRID 1664503ノート

反応式

HRID 1664503 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
75 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-82b3a3842615437fb9898c4652d3eb45
出典データセット
uspto-grants-2011_10
特許番号
US08039478B2

反応ノート

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