Sodium Dithionite → 7,8-Dihydropteridine

HRID 616252ノート

反応式

HRID 616252 の反応式
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

参加物

5

反応物 3

HCID 24489Sodium DithioniteHCID 21880558HCID 21880558、化合物HCID 178446283HCID 178446283、化合物

生成物 1

HCID 189641747,8-Dihydropteridine収率 70.3%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-bd3aa916ab024ab4b6a80a9e33b69739
出典データセット
uspto-grants-1978_02
特許番号
US04073786

反応ノート

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