Ethanol → HCID 18982127、化合物

HRID 1463270ノート

反応式

HRID 1463270 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-58dde71edb604443b4dadfbdca11efed
出典データセット
uspto-grants-1994_04
特許番号
US05300509

反応ノート

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