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Pyridine → 2-[2-(tert-Butyl-dimethyl-silanyloxy)-ethyl]-(5-tert-butyl-2H-pyrazol-3-yl)-carbamic acid 2,2,2-trichloro-ethyl ester

HRID 1446654
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HRID 1446654 반응식
[C:1]([C:5]1[CH:6]=[C:7]([NH2:20])[N:8]([CH2:10][CH2:11][O:12][Si:13]([C:16]([CH3:19])([CH3:18])[CH3:17])([CH3:15])[CH3:14])[N:9]=1)([CH3:4])([CH3:3])[CH3:2].N1C=CC=CC=1.Cl[C:28]([O:30][CH2:31][C:32]([Cl:35])([Cl:34])[Cl:33])=[O:29].C(OCC)(=O)C>C1COCC1.O>[Cl:33][C:32]([Cl:35])([Cl:34])[CH2:31][O:30][C:28](=[O:29])[NH:20][C:7]1[N:8]([CH2:10][CH2:11][O:12][Si:13]([C:16]([CH3:19])([CH3:18])[CH3:17])([CH3:14])[CH3:15])[N:9]=[C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[CH:6]=1
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HCID 1049PyridineHCID 8857Ethyl AcetateHCID 870632,2,2-Trichloroethyl chloroformateHCID 685465445-tert-Butyl-2-[2-(tert-butyl-dimethyl-silanyloxy)-ethyl]-2H-pyrazol-3-ylamine

생성물 1

HCID 685422102-[2-(tert-Butyl-dimethyl-silanyloxy)-ethyl]-(5-tert-butyl-2H-pyrazol-3-yl)-carbamic acid 2,2,2-trichloro-ethyl ester수율 100%

시약·촉매·용매

2
HCID 962Water용매HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

Dissolve 5-tert-butyl-2-[2-(tert-butyl-dimethyl-silanyloxy)-ethyl]-2H-pyrazol-3-ylamine (5.5 g, 0.018 mol) in THF (100 mL) under N2 and cool to 0° C. Add pyridine (1.6 mL, 1.1 equiv.) via syringe followed by dropwise addition of 2,2,2-trichloroethyl chloroformate (2.7 mL, 1.1 equiv.). Stir the reaction at 0° C. for one hour then remove the cooling bath and allow the reaction to stir for a total of 5 hours. Dilute the reaction with ethyl acetate and water. Wash the organic layer with water then saturated aqueous saturated sodium chloride and then dry over magnesium sulfate, filter, and concentrate in vacuo to give a residue (8.7 g, 100%) that is used without further purification. MS (ES), m/z 474 (M+1).

후처리

  1. customthe reaction at 0° C. for one hour
  2. customthen remove the cooling bath
  3. customthe reaction
  4. stirringto stir for a total of 5 hours
  5. additionDilute
  6. washWash the organic layer with water
  7. dry with materialsaturated aqueous saturated sodium chloride and then dry over magnesium sulfate
  8. filtrationfilter
  9. concentrationconcentrate in vacuo

출처 및 근거

ORD 기록
ord-1cc696cb95e44dee9e7e38a7c65012dd
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07666879B2

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