Ethanol → HCID 18982127、化合物

HRID 1440884ノート

反応式

HRID 1440884 の反応式
[NH2:1][C:2]1[C:7]([N:8]=O)=[C:6]([NH2:10])[N:5]=[C:4]([NH:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)[N:3]=1.C(O)C.S(S([O-])=O)([O-])=O.[Na+].[Na+]>O>[CH3:21][O:20][C:17]1[CH:18]=[CH:19][C:14]([CH2:13][CH2:12][NH:11][C:4]2[N:3]=[C:2]([NH2:1])[C:7]([NH2:8])=[C:6]([NH2:10])[N:5]=2)=[CH:15][CH:16]=1

参加物

5

反応物 3

HCID 702EthanolHCID 24489Sodium DithioniteHCID 18982108HCID 18982108、化合物

生成物 1

HCID 18982127HCID 18982127、化合物収率 64.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 4,6-diamino-2-[2-(4-methoxyphenyl)-ethyl]amino-5-nitrosopyrimidine (13.3 g), absolute ethanol (150 ml) and water (150 ml) was heated almost to reflux. Sodium dithionite was added slowly, portionwise until the red colour disappeared. The mixture was filtered hot. After cooling the solid was removed by filtration, triturated with isopropyl alcohol, and dried to give 2-[2-(4-methoxyphenyl)ethyl]amino-4,5,6-triaminopyrimidine as a solid (8.2 g) m.p. 134°-138° C.; NMR: DMSO-d6 ; 2.65-2.85(t, 2H, CH2 --CH2), 3.25-3.5(t, 2H, CH2 -NH),3.7(s, 3H, OCH3), 6.45-6.65 (b, 2H, NH2), 6.7-6.85(b, 1H, NH), 6.8-6.9 (d,2H, aromatic-H), 7.1-7.25(d,2H, aromatic-H). Also 2.8-4.0 (v.br, 4H, 2×NH2).

後処理

  1. temperaturewas heated almost
  2. temperatureto reflux
  3. filtrationThe mixture was filtered hot
  4. temperatureAfter cooling the solid
  5. customwas removed by filtration
  6. customtriturated with isopropyl alcohol
  7. customdried

出典と根拠

ORDレコード
ord-c4150f4ac9944f6a9e333259503d3ac5
出典データセット
uspto-grants-1996_03
特許番号
US05500428

反応ノート

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