Sodium Hydroxide → HCID 135735686, 화합물

HRID 28233노트

반응식

HRID 28233 반응식
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

참가 물질

3

반응물 2

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

생성물 1

HCID 135735686HCID 135735686, 화합물수율 76%

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-78b957fcf06e4428af9ab67c3309cf6a
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04225710

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