Hydrochloric Acid → 2-(3-bromo-1H-pyrazol-1-yl)ethan-1-ol

HRID 2090391노트

반응식

HRID 2090391 반응식
[CH3:1][C:2](C)([O-:4])C.[K+].C1COCC1.[Br:12][C:13]1[CH:17]=[CH:16][NH:15][N:14]=1.O1CCOS1(=O)=O.Cl>CN(C=O)C.C(OCC)(=O)C>[Br:12][C:13]1[CH:17]=[CH:16][N:15]([CH2:1][CH2:2][OH:4])[N:14]=1

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 140751,3,2-Dioxathiolane, 2,2-dioxideHCID 23665647Potassium tert-butoxideHCID 178419412HCID 178419412, 화합물

생성물 1

HCID 594022992-(3-bromo-1H-pyrazol-1-yl)ethan-1-ol

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

Potassium tert-butoxide in THF (0.510 mL, 0.510 mmol) was added to a solution of 3-bromo-1H-pyrazole (50.0 mg, 0.340 mmol) in DMF (3 mL) and stirred at r.t. for 10 min, and then 1,3,2-dioxathiolane 2,2-dioxide (0.0633 g, 0.510 mmol) was added and the stirred at r.t. for 1 h. At this time, conc. HCl (0.3 mL) was added to the above reaction mixture and then stirred at r.t. overnight. The mixture was diluted with ethyl acetate, washed with saturated NaHCO3, water and brine, dried over Na2SO4, filtered, and concentrated to give the crude product which was directly used in the next reaction without further purification. LCMS (M+H)+: m/z=191.0.

후처리

  1. stirringthe stirred at r.t. for 1 h
  2. stirringstirred at r.t. overnight
  3. washwashed with saturated NaHCO3, water and brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ddab1f1833374d4f9d20640487b75a10
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08436008B2

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