Formate → HCID 12849808, 화합물

HRID 746208노트

반응식

HRID 746208 반응식
C([O-])=O.[CH3:4][O:5][C:6]1[CH:15]=[CH:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]=1[OH:16].[NH2:17][C:18]1[N:23]=[C:22]([NH2:24])[C:21]([CH2:25]O)=[CH:20][N:19]=1.Cl>C(O)(=O)C>[NH2:17][C:18]1[N:23]=[C:22]([NH2:24])[C:21]([CH2:25][C:14]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7]([OH:16])=[C:6]([O:5][CH3:4])[CH:15]=2)=[CH:20][N:19]=1

참가 물질

6

반응물 4

HCID 283FormateHCID 313Hydrochloric AcidHCID 2958782,4-Diamino-5-pyrimidinemethanolHCID 109975355-Hydroxy-6-methoxynaphthalene

생성물 1

HCID 12849808HCID 12849808, 화합물수율 31.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

The formate of 2-methoxy-1-naphthol (J. E. Oatis, Jr., M. P. Russell, D. R. Knapp and T. Walle, J. Med. Chem. 1981, 24, 309) (7.23 g, 30.3 mmol), 2,4-diamino-5-hydroxymethylpyrimidine (4.35 g, 30.3 mmol), concentrated hydrochloric acid (4.2 mL) and glacial acetic acid (60 mL) were refluxed 2 hr. The resulting dark solution was evaporated to dryness and the residue dissolved in water and neutralized with ammonia. The resulting tan precipitate (5.2 g) was recrystallized from aqueous ethanol containing a slight excess of hydrochloric acid to give title compound as tan powder (2.83 g, 28%); mp ca. 290°-300° dec. Anal. Calcd for C16H16N4O2.HCl: C, 57.75; H, 5.15; N, 16.84; Cl, 10.65. Found: C, 57.62; H, 5.21; N, 16.79; Cl, 10.61.

후처리

  1. customThe resulting dark solution was evaporated to dryness
  2. dissolutionthe residue dissolved in water and neutralized with ammonia
  3. customThe resulting tan precipitate (5.2 g) was recrystallized from aqueous ethanol containing a slight excess of hydrochloric acid

출처 및 근거

ORD 기록
ord-dd3f29c8c78b48d8a296536706b9f3d8
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04603136

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