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

Tributyltin Chloride → 7-(Pyridin-3-yl)carbonyl-2-(tri-n-butylstannyl)imidazo[5,1-b]thiazole

HRID 1072324
노트
인쇄 미리보기

반응식

HRID 1072324 반응식
[CH2:1]([Sn:5](Cl)([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].C[Si]([N-][Si](C)(C)C)(C)C.[Li+].C1COCC1.[N:30]1[CH:35]=[CH:34][CH:33]=[C:32]([C:36]([C:38]2[N:39]=[CH:40][N:41]3[CH:45]=[CH:44][S:43][C:42]=23)=[O:37])[CH:31]=1.[Cl-].[NH4+]>C1COCC1>[N:30]1[CH:35]=[CH:34][CH:33]=[C:32]([C:36]([C:38]2[N:39]=[CH:40][N:41]3[CH:45]=[C:44]([Sn:5]([CH2:10][CH2:11][CH2:12][CH3:13])([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:1][CH2:2][CH2:3][CH3:4])[S:43][C:42]=23)=[O:37])[CH:31]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 15096Tributyltin ChlorideHCID 25517Ammonium ChlorideHCID 223903557-(Pyridin-3-yl)carbonylimidazo[5,1-b]thiazoleHCID 23714775LiHMDS tetrahydrofuran3회

생성물 1

HCID 223903847-(Pyridin-3-yl)carbonyl-2-(tri-n-butylstannyl)imidazo[5,1-b]thiazole

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

반응 조건

온도
-50 °C

실험 절차

Tri-n-butylstannyl chloride (0.841 ml) and 2.95 ml of a 1.0 N lithium bis(trimethylsilyl)amide/THF solution were added to a solution of 520 mg of 7-(pyridin-3-yl)carbonylimidazo[5,1-b]thiazole in 25 ml of THF at −60° C. under an argon atmosphere, and the mixture was stirred for 20 min. The temperature of the mixture was raised to −50° C., 1.0 ml of a 1.0 N lithium bis(trimethylsilyl)amide/THF solution was added thereto, and the mixture was stirred for 30 min. The temperature of the mixture was raised to −40° C., 0.5 ml of a 1.0 N lithium bis(trimethylsilyl)amide/THF solution was added thereto, and the mixture was stirred for 30 min. An aqueous ammonium chloride solution was added to the reaction solution, and the mixture was extracted with ethyl acetate, followed by washing with brine. The organic layer was dried over anhydrous magnesium sulfate. The solvent was then removed by distillation, and the residue was purified by column chromatography on silica gel (hexane:ethyl acetate=2:1→ethyl acetate only) to give 712 mg of the title compound.

후처리

  1. stirringthe mixture was stirred for 30 min
  2. temperatureThe temperature of the mixture was raised to −40° C.
  3. stirringthe mixture was stirred for 30 min
  4. extractionthe mixture was extracted with ethyl acetate
  5. washby washing with brine
  6. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  7. customThe solvent was then removed by distillation
  8. customthe residue was purified by column chromatography on silica gel (hexane

출처 및 근거

ORD 기록
ord-2001be10c4314a4a95c5fde4c48fadd7
출처 데이터셋
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06908913B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트