Hydrochloric Acid → HCID 13565136, 화합물

HRID 1248890노트

반응식

HRID 1248890 반응식
[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]

참가 물질

8

반응물 5

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

생성물 1

HCID 13565136HCID 13565136, 화합물수율 83%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7e2552c3f6844bee940844d27853980c
출처 데이터셋
uspto-grants-1986_12
특허 번호
US04627871

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