홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Hydrochloric Acid → (1-methyl-1H-pyrazol-5-yl)boronic acid

HRID 46337
노트
인쇄 미리보기

반응식

HRID 46337 반응식
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[N:3]1.C([Li])CCC.[B:12](OC(C)C)([O:17]C(C)C)[O:13]C(C)C.Cl>O1CCCC1>[CH3:1][N:2]1[C:6]([B:12]([OH:17])[OH:13])=[CH:5][CH:4]=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 21531Triisopropyl borateHCID 702551H-Pyrazole, 1-methyl-HCID 178418339Butyllithium

생성물 1

HCID 11182610(1-methyl-1H-pyrazol-5-yl)boronic acid수율 33%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 1-methyl-1H-pyrazole (2.49 mL, 30 mmol) in tetrahydrofuran (100 mL) was added butyllithium (2.5 M in hexane, 15.6 mL, 39 mmol) at −78° C. dropwise. After stirring for 1 hour, triisopropyl borate (27.6 mL, 120 mmol) was added and the reaction mixture was gradually warmed to room temperature for 16 hours. Hydrochloric acid (1 N aqueous solution) was added to the reaction mixture until pH 7 achieved. The mixture was extracted with dichloromethane:methanol (9:1, 5×200 mL). Combined organic extracts were dried over magnesium sulphate and concentrated in vacuo to obtain crude residue. Purification was undertaken by flash column chromatography (ISCO™) eluting with dichloromethane:methanol (7:3, by volume) to afford the title compound as a white solid, 1258 mg, 33% yield.

후처리

  1. extractionThe mixture was extracted with dichloromethane:methanol (9:1, 5×200 mL)
  2. dry with materialCombined organic extracts were dried over magnesium sulphate
  3. concentrationconcentrated in vacuo
  4. customto obtain crude residue
  5. customPurification
  6. washeluting with dichloromethane:methanol (7:3, by volume)

출처 및 근거

ORD 기록
ord-d10a93e5238f4cc7a481ac6945dcec4e
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08541588B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트