Ethanol → HCID 18982127, 화합물

HRID 1463270노트

반응식

HRID 1463270 반응식
[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

참가 물질

5

반응물 3

HCID 702EthanolHCID 24489Sodium DithioniteHCID 18982108HCID 18982108, 화합물

생성물 1

HCID 18982127HCID 18982127, 화합물수율 64.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-58dde71edb604443b4dadfbdca11efed
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05300509

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