Hydrochloric Acid → HCID 13565136、化合物

HRID 1248890ノート

反応式

HRID 1248890 の反応式
[CH3:1][O:2][C:3]([CH3:8])([CH3:7])[C:4](O)=[O:5].C(N(CC)CC)C.[Cl-].C(OC(=O)O)C.[NH2:23][C:24]1[CH:29]=[CH:28][C:27]([S:30][C:31]2[N:36]=[C:35]([CH3:37])[CH:34]=[C:33]([CH3:38])[N:32]=2)=[CH:26][CH:25]=1.Cl>O1CCCC1.O>[CH3:1][O:2][C:3]([CH3:8])([CH3:7])[C:4]([NH:23][C:24]1[CH:25]=[CH:26][C:27]([S:30][C:31]2[N:32]=[C:33]([CH3:38])[CH:34]=[C:35]([CH3:37])[N:36]=2)=[CH:28][CH:29]=1)=[O:5]

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 27374774-((4,6-Dimethylpyrimidin-2-yl)thio)anilineHCID 98554652-Methoxy-2-methylpropanoic acidHCID 86741142HCID 86741142、化合物

生成物 1

HCID 13565136HCID 13565136、化合物収率 83%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

11.8 g (0.1 mole) of α-methoxy-isobutyric acid were dissolved in 150 ml of tetrahydrofuran, and 10.1 g (0.1 mole) of triethylamine were added. 10.85 g (0.1 mole) of carbonic acid ethyl ester-chloride were added dropwise at 10°-15° C., with stirring. The mixture was subsequently stirred at room temperature for 2 hours and 23.1 g (0.1 mole) of 2-(4-aminophenylmercapto)-4,6-dimethyl-pyrimidine were then added in portions. The mixture was subsequently stirred at room temperature for 1 hour and boiled under reflux for a further 2 hours. The reaction mixture was cooled and then stirred into one liter of water rendered slightly acid with hydrochloric acid. The crystals precipitated were filtered off with suction, washed with water and dried in air. 27.4 g (83% of theory) of 2-(4-(α-methoxy-isobutyrylamino)-phenylmercapto)-4,6-dimethyl-pyrimidine were obtained.

後処理

  1. stirringThe mixture was subsequently stirred at room temperature for 2 hours
  2. stirringThe mixture was subsequently stirred at room temperature for 1 hour
  3. temperatureunder reflux for a further 2 hours
  4. temperatureThe reaction mixture was cooled
  5. customThe crystals precipitated
  6. filtrationwere filtered off with suction
  7. washwashed with water
  8. customdried in air

出典と根拠

ORDレコード
ord-7e2552c3f6844bee940844d27853980c
出典データセット
uspto-grants-1986_12
特許番号
US04627871

反応ノート

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