Hydrochloric Acid → 4(1H)-Pyrimidinone, 3-(2,6-dimethylphenyl)-1-ethyltetrahydro-2-thioxo-

HRID 2393328노트

반응식

HRID 2393328 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][C:10](=[S:19])[N:11]([CH2:14][CH2:15][C:16](O)=[O:17])[CH2:12][CH3:13].Cl>CC(C)=O>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]1[C:16](=[O:17])[CH2:15][CH2:14][N:11]([CH2:12][CH3:13])[C:10]1=[S:19]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 18975625HCID 18975625, 화합물

생성물 1

HCID 113115614(1H)-Pyrimidinone, 3-(2,6-dimethylphenyl)-1-ethyltetrahydro-2-thioxo-수율 47.2%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

3-[3-(2,6-dimethylphenyl)-1-ethyl-thioureido]propionic acid (12 g) was dissolved in acetone (245 mL). Conc. HCl (5 mL) was added and the mixture was heated at reflux for 18 hours. The reaction mixture was evaporated to dryness. The residue was dissolved in methylene chloride (100 mL), and washed with 1N NaOH. The organic phase was dried over anhydrous magnesium sulfate, then evaporated to dryness. The solid was recrystallized from ethyl acetate to give the title compound (5.3 g) as a white solid, m.p. 124°-126° C.

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 18 hours
  3. customThe reaction mixture was evaporated to dryness
  4. dissolutionThe residue was dissolved in methylene chloride (100 mL)
  5. washwashed with 1N NaOH
  6. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  7. customevaporated to dryness
  8. customThe solid was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-04600c432d684dc08cc38c7b1c728ebe
출처 데이터셋
uspto-grants-1998_09
특허 번호
US05807864

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