Sodium Hydroxide → HCID 135735686、化合物

HRID 1065253ノート

反応式

HRID 1065253 の反応式
N[C:2]1[C:11]2[C:10](=[O:12])[C:9]([CH3:13])=[N:8][N:7]([CH3:14])[C:6]=2[N:5]=[C:4]([NH2:15])[N:3]=1.[OH-:16].[Na+]>>[NH2:15][C:4]1[NH:3][C:2](=[O:16])[C:11]2[C:10](=[O:12])[C:9]([CH3:13])=[N:8][N:7]([CH3:14])[C:6]=2[N:5]=1

参加物

3

反応物 2

HCID 14798Sodium HydroxideHCID 124630735,7-diamino-1,3-dimethylpyrimido(4,5-c)pyridazin-4(1H)-one

生成物 1

HCID 135735686HCID 135735686、化合物収率 76%

実験手順

A mixture of 5,7-diamino-1,3-dimethylpyrimido(4,5-c)pyridazin-4(1H)-one (0.50 g) and 1.5 N aqueous sodium hydroxide (35 ml) was stirred at reflux for 24 hours after which time a small amount of solid was removed by filtration of the hot mixture. On cooling, the yellow filtrate deposited white needles which were collected by filtration and dissolved in warm water (20 ml). Adjustment of this aqueous solution to pH 5 by dropwise addition of 6 N hydrochloric acid and subsequent cooling to room temperature provided a very finely divided white precipitate which was collected, washed with water and dried under vacuum at 70° C. to give 7-amino-1,3-dimethylpyrimido(4,5-c)pyridazine-4,5(1H, 6H)-dione (0.38 g; 76% of theoretical yield). The u.v., i.r., and n.m.r. spectra of this compound were identical to those of the sample made according to the procedure of Example 2.

後処理

  1. temperatureat reflux for 24 hours after which time a small amount of solid
  2. customwas removed by filtration of the hot mixture
  3. temperatureOn cooling
  4. filtrationwere collected by filtration
  5. dissolutiondissolved in warm water (20 ml)
  6. additionAdjustment of this aqueous solution to pH 5 by dropwise addition of 6 N hydrochloric acid
  7. customprovided a very finely divided white precipitate which
  8. customwas collected
  9. washwashed with water
  10. customdried under vacuum at 70° C.

出典と根拠

ORDレコード
ord-b6e30d69dfa5444bb06495e53d19e369
出典データセット
uspto-grants-1982_05
特許番号
US04329362

反応ノート

読み込み中…