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

N,N,N',N'-Tetramethylethylenediamine → 2-((Phenylmethoxy)methyl)-5-(tributylstannyl)-2H-tetrazole

HRID 1016180
노트
인쇄 미리보기

반응식

HRID 1016180 반응식
[CH2:1]([O:8][CH2:9][N:10]1[N:14]=[N:13][CH:12]=[N:11]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN(C)CCN(C)C.C([Li])CCC.[CH2:28]([Sn:32](Cl)([CH2:37][CH2:38][CH2:39][CH3:40])[CH2:33][CH2:34][CH2:35][CH3:36])[CH2:29][CH2:30][CH3:31]>C(OCC)C>[CH2:1]([O:8][CH2:9][N:10]1[N:14]=[N:13][C:12]([Sn:32]([CH2:33][CH2:34][CH2:35][CH3:36])([CH2:37][CH2:38][CH2:39][CH3:40])[CH2:28][CH2:29][CH2:30][CH3:31])=[N:11]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 15096Tributyltin ChlorideHCID 107263402-((benzyloxy)methyl)-2H-tetrazoleHCID 178418339Butyllithium

생성물 1

HCID 113405612-((Phenylmethoxy)methyl)-5-(tributylstannyl)-2H-tetrazole수율 60%

시약·촉매·용매 1

HCID 3283
Diethyl Ether
용매
2회

반응 조건

온도
-78 °C

실험 절차

In a flame-dried three-neck flask, a solution of 2-(benzyloxymethyl)-2H-tetrazole (2.01 g, 10.57 mmol) and tetramethylethylenediamine (3.16 mL, 21.4 mmol) in diethyl ether (30 mL) was cooled to −78° C. and treated with the dropwise addition of n-butyllithium (1.6 M in hexanes, 7.3 mL, 11.62 mmol), causing the color of the solution to turn dark red. The mixture was stirred for 10 minutes, then transferred via canulus to a solution of tributyltin chloride (2.9 mL, 10.57 mmol) in diethyl ether (20 mL) which had been pre-cooled to −78° C. The reaction was stirred for 45 minutes, then quenched with saturated ammonium chloride solution. The mixture was allowed to come to room temperature, and the layers were separated. The aqueous phase was extracted 3× with ethyl acetate, and the combined organic phases were washed with brine, dried over sodium sulfate, and concentrated in-vacuo. The residue was purified over silica gel, eluting with 1% then 5% then 10% ethyl acetate/hexanes to yield the title compound (3.0 g, 60% yield) as a colorless oil.

후처리

  1. stirringThe reaction was stirred for 45 minutes
  2. customquenched with saturated ammonium chloride solution
  3. customto come to room temperature
  4. customthe layers were separated
  5. extractionThe aqueous phase was extracted 3× with ethyl acetate
  6. washthe combined organic phases were washed with brine
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated in-vacuo
  9. customThe residue was purified over silica gel
  10. washeluting with 1%

출처 및 근거

ORD 기록
ord-d3a94fdbd36e4793af227d015fd00ea3
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07985861B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트