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N,N,N',N'-Tetramethylethylenediamine → 2-(Tributylstannyl)-1-benzofuran-5-carbaldehyde

HRID 506191
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HRID 506191 반응식
CN1CCNCC1.[Li]CCCC.[O:13]1[C:17]2[CH:18]=[CH:19][C:20]([CH:22]=[O:23])=[CH:21][C:16]=2[CH:15]=[CH:14]1.CN(C)CCN(C)C.[CH2:32]([Sn:36](Cl)([CH2:41][CH2:42][CH2:43][CH3:44])[CH2:37][CH2:38][CH2:39][CH3:40])[CH2:33][CH2:34][CH3:35]>CCCCCC.C1COCC1>[CH2:41]([Sn:36]([CH2:32][CH2:33][CH2:34][CH3:35])([CH2:37][CH2:38][CH2:39][CH3:40])[C:14]1[O:13][C:17]2[CH:18]=[CH:19][C:20]([CH:22]=[O:23])=[CH:21][C:16]=2[CH:15]=1)[CH2:42][CH2:43][CH3:44]
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참가 물질

8

반응물 5

HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 15096Tributyltin ChlorideHCID 531671-MethylpiperazineHCID 27738751-Benzofuran-5-carbaldehydeHCID 178418339Butyllithium2회

생성물 1

HCID 866168342-(Tributylstannyl)-1-benzofuran-5-carbaldehyde수율 34%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8058Hexane용매

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온도
0 °C

실험 절차

To a solution of N-methylpiperazine (0.75 g, 7.5 mmol) in hexane (15 mL) at 0° C. under nitrogen was added dropwise a solution of n-BuLi (3 mL, 7.43 mmol, 2.5M/hexanes), and the reaction mixture was stirred at 0° C. for 40 min. 1-Benzofuran-5-carbaldehyde (1.0 g, 6.8 mmol) was added dropwise to the reaction mixture at 0° C. and the resulting mixture was stirred at 0° C. for 15 min. After addition of tetramethylethylenediamine (TMEDA) (1.7 g, 14.96 mmol), a solution of n-BuLi (6.0 mL, 14.86 mmol, 2.5M/hexanes) was added dropwise to the reaction mixture at 0° C. and the reaction mixture was allowed to warm up to room temperature and stirred for a total of 18 h. After the reaction mixture was cooled to 0° C. and THF (30 mL) was added, the reaction mixture was cooled to −50° C., tributyltin chloride (4.87 g, 14.96 mmol) was added dropwise, and the reaction mixture was stirred at −50° C. for 15 min. and at room temperature for 5-6 h. The reaction mixture was quenched with saturated aqueous NaHCO3 and extracted into diethyl ether. The organic layer was dried over sodium sulfate and concentrated and the crude product was purified by column chromatography (ethyl acetate/hexane, 2%) to give 1.0 g (34%) of 2-(tributylstannyl)-1-benzofuran-5-carbaldehyde as a yellow oil.

후처리

  1. stirringthe resulting mixture was stirred at 0° C. for 15 min
  2. temperatureto warm up to room temperature
  3. stirringstirred for a total of 18 h
  4. temperatureAfter the reaction mixture was cooled to 0° C.
  5. temperaturethe reaction mixture was cooled to −50° C.
  6. stirringthe reaction mixture was stirred at −50° C. for 15 min. and at room temperature for 5-6 h
  7. customThe reaction mixture was quenched with saturated aqueous NaHCO3
  8. extractionextracted into diethyl ether
  9. dry with materialThe organic layer was dried over sodium sulfate
  10. concentrationconcentrated
  11. customthe crude product was purified by column chromatography (ethyl acetate/hexane, 2%)

출처 및 근거

ORD 기록
ord-f045eb7bde9240b8a2c6d4b6b3a1e309
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07781591B2

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