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

HRID 2393328ノート

反応式

HRID 2393328 の反応式
[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]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 18975625HCID 18975625、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-04600c432d684dc08cc38c7b1c728ebe
出典データセット
uspto-grants-1998_09
特許番号
US05807864

反応ノート

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