Sodium Hydroxide → HCID 178458744, 화합물

HRID 1579251노트

반응식

HRID 1579251 반응식
[CH3:1][N:2]([CH3:11])[C:3]1[N:8]=[C:7]([OH:9])[CH:6]=[C:5]([OH:10])[N:4]=1.[OH-].[Na+].[CH2:14](OS(C1C=CC(C)=CC=1)(=O)=O)[CH2:15][CH3:16]>C(O)(=O)C>[CH3:1][N:2]([CH3:11])[C:3]1[N:4]=[C:5]([O:10][CH2:14][CH2:15][CH3:16])[CH:6]=[C:7]([OH:9])[N:8]=1

참가 물질

5

반응물 3

HCID 14798Sodium Hydroxide2회HCID 69035Propyl p-toluenesulfonateHCID 178483102HCID 178483102, 화합물

생성물 1

HCID 178458744HCID 178458744, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

124 g (0.8 mol) of 2-dimethylamino-4,6-dihydroxypyrimidine are stirred with 800 cc of 1N sodium hydroxide solution at 60° for 1 hour. 171 g (0.8 mol) of p-toluenesulphonic acid-n-propyl ester are added dropwise at 90° over the course of 1 hour and the pH is kept at 8-8.5 by the dropwise addition of 1N sodium hydroxide solution. The mixture is stirred at 90° for 16 hours, cooled to 5°, neutralized with glacial acetic acid and allowed to stand at room temperature for 6 hours. The precipitated crystals are subsequently filtered by suction, washed with water, dissolved in approximately 700 cc of chloroform, dried over sodium sulphate and evaporated to dryness in a vacuum. The residue is decomposed with 500 cc of petroleum ether, filtered by suction and recrystallized from benzene, washed with petroleum ether and dried at 60° in a high vacuum. M.P.: 194°-195°.

후처리

  1. temperaturecooled to 5°
  2. waitto stand at room temperature for 6 hours
  3. filtrationThe precipitated crystals are subsequently filtered by suction
  4. washwashed with water
  5. dissolutiondissolved in approximately 700 cc of chloroform
  6. dry with materialdried over sodium sulphate
  7. customevaporated to dryness in a vacuum
  8. filtrationfiltered by suction
  9. customrecrystallized from benzene
  10. washwashed with petroleum ether
  11. customdried at 60° in a high vacuum

출처 및 근거

ORD 기록
ord-c80f439114a849bd84ed6092115aca65
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03931180

반응 노트

불러오는 중…