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Tert-Butanesulfinamide → HCID 178455565, 화합물

HRID 522163
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HRID 522163 반응식
[NH:1]1[CH:5]=[C:4]([CH:6]=O)[N:3]=[N:2]1.[CH3:8][C:9]([S:12]([NH2:14])=[O:13])([CH3:11])[CH3:10]>O1CCCC1.CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].[Ti+4]>[NH:1]1[CH:5]=[C:4]([CH:6]=[N:14][S:12]([C:9]([CH3:11])([CH3:10])[CH3:8])=[O:13])[N:3]=[N:2]1
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참가 물질

5

반응물 2

HCID 3382465Tert-ButanesulfinamideHCID 178519887HCID 178519887, 화합물

생성물 1

HCID 178455565HCID 178455565, 화합물수율 98%

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매HCID 8028Tetrahydrofuran용매

실험 절차

1H-1,2,3-triazole-4-carbaldehyde (1 g, 10.3 mmol) and 2-methylpropane-2-sulfinamide (1.25 g, 10.3 mmol) were dissolved in tetrahydrofuran (20 mL). Titanium tetraisopropoxide (3.1 mL, 10.5 mmol) was added and the reaction heated at reflux for 8 hours. After cooling to room temperature, the reaction was quenched by adding saturated aqueous sodium chloride solution (5 mL) followed by dilution with tetrahydrofuran (80 mL) and stirred for 30 minutes. The mixture was filtered through a pad of Arbocel and the filtrate concentrated in vacuo, azeotroping with THF to afford the title compound (2.02 g, 98%).

후처리

  1. temperaturethe reaction heated
  2. temperatureat reflux for 8 hours
  3. customthe reaction was quenched
  4. additionby adding saturated aqueous sodium chloride solution (5 mL)
  5. filtrationThe mixture was filtered through a pad of Arbocel
  6. concentrationthe filtrate concentrated in vacuo
  7. customazeotroping with THF

출처 및 근거

ORD 기록
ord-49689f2ca671408b997a6dc9f06b17a4
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09328096B2

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