Cyanamide → HCID 178486952, 화합물

HRID 522480

반응식

HRID 522480 반응식
[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([O:9][CH3:10])[CH:3]=1.[N:11]#[C:12][NH2:13]>Cl.O>[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][C:12]([NH2:13])=[NH:11])=[C:4]([O:9][CH3:10])[CH:3]=1

참가 물질

5

반응물 2

HCID 9864CyanamideHCID 4592574-Bromo-2-methoxyaniline

생성물 1

HCID 178486952HCID 178486952, 화합물수율 99.2%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

To a solution of 4-bromo-2-methoxyaniline 7.1 g (35.1 mmol) in HCl 25% m/v 20 mL, cyanamide 20.6 g (494.3 mmol) was added in portion (1.6 g every half hour). The reaction was stirred at 60° C. for 6 hours, then cooled down to room temperature, diluted with H2O (20 mL), extracted with AcOEt (10 mL). NaOH 35% (30 mL) was added to pH>>14. The aqueous phase was extracted with AcOEt (3×50 mL), dried over Na2SO4 and concentrated to afford 8.5 g (quantitative yield) of the title compound.

후처리

  1. temperaturecooled down to room temperature
  2. extractionextracted with AcOEt (10 mL)
  3. additionNaOH 35% (30 mL) was added
  4. extractionThe aqueous phase was extracted with AcOEt (3×50 mL)
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d6a4464abc364f4787907a8e4c53f034
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09333205B2

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