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Cyanamide → 5-tert-Butyl-1,3-thiazol-2-amine

HRID 78494
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HRID 78494 반응식
[CH3:1][C:2]([CH3:7])([CH3:6])[CH2:3][CH:4]=O.N1CCCC1.O.C1(C)C=CC([S:20](O)(=O)=O)=CC=1.[N:25]#[C:26][NH2:27]>C1CCCCC1>[C:2]([C:3]1[S:20][C:26]([NH2:27])=[N:25][CH:4]=1)([CH3:7])([CH3:6])[CH3:1]
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참가 물질

6

반응물 4

HCID 9864CyanamideHCID 31268PyrrolidineHCID 763353,3-DimethylbutanalHCID 521998p-Toluenesulfonic acid monohydrate

생성물 1

HCID 6764855-tert-Butyl-1,3-thiazol-2-amine

시약·촉매·용매 1

HCID 8078Cyclohexane용매

실험 절차

To a solution of 3,3-dimethylbutyraldehyde (10 g, 99.8 mmol) in 200 mL of cyclohexane was added pyrrolidine (8.7 mL, 0.11 mol) followed by p-toluenesulfonic acid monohydrate (0.95 g, 5.0 mmol). This reaction flask was equipped with a Dean-Stark trap and the mixture was warmed to reflux and was allowed to stir for 3 hours. The mixture was cooled to ambient temperature, filtered and concentrated under reduced pressure. The residue was dissolved in 75 mL of CH3OH, sulfur was added (3.2 g, 99.8 mmol), and the mixture was cooled to 0° C. Cyanamide (4.2 g, 99.8 mmol) was added portion wise over 10 minutes and the mixture was allowed to warm to ambient temperature and stir for 18 hours. The reaction mixture was concentrated under reduced pressure and purified by column chromatography (SiO2, ethyl acetate then 10% methanol in ethyl acetate) to afford the title compound. MS (DCI/NH3) m/z 157 (M+H)+.

후처리

  1. customThis reaction flask was equipped with a Dean-Stark trap
  2. temperaturethe mixture was warmed
  3. temperatureto reflux
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. dissolutionThe residue was dissolved in 75 mL of CH3OH
  7. additionsulfur was added (3.2 g, 99.8 mmol)
  8. temperaturethe mixture was cooled to 0° C
  9. temperatureto warm to ambient temperature
  10. stirringstir for 18 hours
  11. concentrationThe reaction mixture was concentrated under reduced pressure
  12. custompurified by column chromatography (SiO2, ethyl acetate

출처 및 근거

ORD 기록
ord-30c90db8f5794c2eb03e0b7f86ce22e9
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08841334B2

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