Formate → HCID 12849808、化合物

HRID 1903839ノート

反応式

HRID 1903839 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 12849808HCID 12849808、化合物収率 31.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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; N, 5.21; N, 16.79; Cl, 10.61.

後処理

  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

出典と根拠

ORDレコード
ord-fddcda81ccf0428bbc07ef5832d3c00c
出典データセット
uspto-grants-1984_03
特許番号
US04438267

反応ノート

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