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

HRID 42544
ノート
印刷プレビュー

反応式

HRID 42544 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283
Diethyl Ether
溶媒
2 回

反応条件

温度
-78 °C

実験手順

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. Once at the prescribed temperature, the mixture was treated with the dropwise addition of n-butyllithium (1.6 M in hexanes, 7.3 mL, 11.62 mmol), which caused the color of the solution to turn dark red. Upon completion of addition, the mixture was stirred for 10 minutes, and then transferred via cannula 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. Upon completion of the transfer, the reaction was stirred for 45 minutes, and then quenched with saturated ammonium chloride solution. The mixture was allowed to come to room temperature, and the aqueous and organic 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 to yield a residue. The residue was purified over silica gel, eluting with 1% then 5% then 10% ethyl acetate/hexanes to yield 2-(benzyloxymethyl)-5-(tributylstannyl)-2H-tetrazole (3.0 g, 60% yield) as a colorless oil.

後処理

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

出典と根拠

ORDレコード
ord-9b74e036973a41e4be89156d2b6cabaf
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08536198B2

反応ノート

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