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

Tributyltin Chloride → 1-Isopropyl-5-tributylstannanyl-1H-pyrazole

HRID 906573
노트
인쇄 미리보기

반응식

HRID 906573 반응식
[Li+].CC([N-]C(C)C)C.[CH:9]([N:12]1[CH:16]=[CH:15][CH:14]=[N:13]1)([CH3:11])[CH3:10].[CH2:17]([Sn:21](Cl)([CH2:26][CH2:27][CH2:28][CH3:29])[CH2:22][CH2:23][CH2:24][CH3:25])[CH2:18][CH2:19][CH3:20]>C1COCC1>[CH:9]([N:12]1[C:16]([Sn:21]([CH2:22][CH2:23][CH2:24][CH3:25])([CH2:26][CH2:27][CH2:28][CH3:29])[CH2:17][CH2:18][CH2:19][CH3:20])=[CH:15][CH:14]=[N:13]1)([CH3:11])[CH3:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 15096Tributyltin ChlorideHCID 2724682Lithium diisopropylamideHCID 134698161-isopropyl-1H-pyrazole

생성물 1

HCID 591645211-Isopropyl-5-tributylstannanyl-1H-pyrazole수율 82%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
-78 °C

실험 절차

To a cold (−78° C.) solution of LDA (prepared from n-BuLi (7.99 mL, 1.6 M, 1.1 eq) and diisopropylamine (1.82 mL, 1.1 eq)) in THF, a solution of 1-isopropyl-1H-pyrazole (1.28 g, 11.6 mmol) in THF was added dropwise while keeping the temperature below −70° C. At the end of the addition, the mixture was stirred at −78° C. for 30 min. Tributyltin chloride (3.44 mL, 1.1 eq) was then added dropwise while keeping the temperature below −70° C. At the end of the addition, the mixture was stirred for 1 h at −78° C. and for 2 h at r.t. The solvent was removed in vacuo and the crude oil was dissolved into AcOEt. The organic phase was washed with water and dried over Na2SO4. The solution was concentrated in vacuo to afford a yellow oil (3.82 g, 82%).

후처리

  1. customthe temperature below −70° C
  2. additionAt the end of the addition
  3. customthe temperature below −70° C
  4. additionAt the end of the addition
  5. stirringthe mixture was stirred for 1 h at −78° C. and for 2 h at r.t
  6. customThe solvent was removed in vacuo
  7. dissolutionthe crude oil was dissolved into AcOEt
  8. washThe organic phase was washed with water
  9. dry with materialdried over Na2SO4
  10. concentrationThe solution was concentrated in vacuo

출처 및 근거

ORD 기록
ord-a0f223fed83c4e4db51374ca18926250
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08012988B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트