Acetic Acid → 4,6-Diaminopyrimidine-2-sulfinic acid

HRID 976944노트

반응식

HRID 976944 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([NH2:8])[N:5]=[C:4]([SH:9])[N:3]=1.OO.C(O)(=[O:14])C.[OH-:16].[Na+]>>[NH2:1][C:2]1[CH:7]=[C:6]([NH2:8])[N:5]=[C:4]([S:9]([OH:14])=[O:16])[N:3]=1

참가 물질

5

반응물 4

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 1785079174,6-diaminopyrimidine-2-thiol

생성물 1

HCID 2438514,6-Diaminopyrimidine-2-sulfinic acid

실험 절차

To a solution of 50 g of 4,6-diamino-2-mercaptopyrimidine (Aldrich, Milwaukee, Wis., USA) in 2N NaOH (220 mL) was added 750 mL of a 3% hydrogen peroxide solution. The solution was maintained at a temperature less than 20° C. Stirring was continued for a further 30 minutes and the clear pale yellow solution was acidified with acetic acid (ca. 50 mL). The precipitate was washed with H2O and air dried, to give 33 as 58 g (95 % yield) of an off-white amorphous acid (m.p. 168°-170° C. decomp.). For analysis, a sample was dissolved in dilute aqueous ammonia and reprecipitated with acetic acid.

후처리

  1. temperatureThe solution was maintained at a temperature less than 20° C
  2. washThe precipitate was washed with H2O and air
  3. customdried

출처 및 근거

ORD 기록
ord-de605518dcb64f55a346b190ae6d938d
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05612468

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