Sodium Dithionite → 7,8-Dihydropteridine

HRID 616252노트

반응식

HRID 616252 반응식
N[C:2]1[N:7]=[C:6](O)[C:5]([N+]([O-])=O)=[C:4]([NH:12][C:13](CC)(CC)[C:14](=[N:17]O)CO)[N:3]=1.S(S([O-])=O)([O-])=O.[Na+].[Na+].N1C2C(=NC=CN=2)C=NC1>[OH-].[Na+]>[N:3]1[C:4]2[NH:12][CH2:13][CH:14]=[N:17][C:5]=2[CH:6]=[N:7][CH:2]=1

참가 물질

5

반응물 3

HCID 24489Sodium DithioniteHCID 21880558HCID 21880558, 화합물HCID 178446283HCID 178446283, 화합물

생성물 1

HCID 189641747,8-Dihydropteridine수율 70.3%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

2-Amino-4-hydroxy-6-(3-hydroxy-2-hydroxyimino-1-spirocyclohexylpropylamino)-5-nitropyrimidine (II) (500 mg) was dissolved in the minimum of 0.1M sodium hydroxide by warming on the steam bath. Sodium dithionite was added portionwise until an almost colourless solution was obtained. On cooling the dihydropteridine separated and was filtered off and purified by dissolving in 2M HCl and reprecipitated by the addition of 0.88 ammonia to pH8. On standing the dihydropteridine (I) (150 mg; yield 38%) was obtained as a pale yellow crystalline solid, m.p. >300 (decomp.).

후처리

  1. temperatureby warming on the steam bath
  2. customwas obtained
  3. customseparated
  4. filtrationwas filtered off
  5. custompurified
  6. dissolutionby dissolving in 2M HCl
  7. customreprecipitated by the addition of 0.88 ammonia to pH8

출처 및 근거

ORD 기록
ord-bd3aa916ab024ab4b6a80a9e33b69739
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04073786

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