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

Benzothiazole → 2-(Tributylstannyl)-1,3-benzothiazole

HRID 1433846
노트
인쇄 미리보기

반응식

HRID 1433846 반응식
[S:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[CH:2]1.C([Li])CCC.[CH2:15]([Sn:19](Cl)([CH2:24][CH2:25][CH2:26][CH3:27])[CH2:20][CH2:21][CH2:22][CH3:23])[CH2:16][CH2:17][CH3:18]>O1CCCC1>[CH2:24]([Sn:19]([CH2:15][CH2:16][CH2:17][CH3:18])([CH2:20][CH2:21][CH2:22][CH3:23])[C:2]1[S:1][C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=1)[CH2:25][CH2:26][CH3:27]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7222BenzothiazoleHCID 15096Tributyltin ChlorideHCID 178418339Butyllithium

생성물 1

HCID 37623922-(Tributylstannyl)-1,3-benzothiazole수율 75.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
-78 °C

실험 절차

To a solution of benzothiazole (30.7 g) in tetrahydrofuran (700 ml), which was cooled at −78° C., was added dropwise n-butyllithium (2.5M solution in hexane) (100 ml) under a nitrogen atmosphere, the solution was stirred for 10 minutes at −78° C. Tributyltin chloride (77.9 g) was added dropwise thereto, the solution was stirred for 1.5 hours at −78° C., and then stirred for 2 hours while warming from −78° C. to room temperature. The reaction mixture was concentrated in vacuo, diethyl ether (400 ml) was added thereto, insoluble material was removed by filtration, and then the solvent was evaporated in vacuo. The residue was purified by distillation in vacuo (0.5 mmHg, 170 to 184° C.) to provide the title compound (73.0 g).

후처리

  1. stirringthe solution was stirred for 1.5 hours at −78° C.
  2. stirringstirred for 2 hours
  3. temperaturewhile warming from −78° C. to room temperature
  4. concentrationThe reaction mixture was concentrated in vacuo, diethyl ether (400 ml)
  5. additionwas added
  6. custominsoluble material was removed by filtration
  7. customthe solvent was evaporated in vacuo
  8. distillationThe residue was purified by distillation in vacuo (0.5 mmHg, 170 to 184° C.)

출처 및 근거

ORD 기록
ord-6cb384d47d4b4554a4e2cddfbf8cda0d
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612114B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트