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

HRID 506191
ノート
印刷プレビュー

反応式

HRID 506191 の反応式
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]
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

8

反応物 5

HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 15096Tributyltin ChlorideHCID 531671-MethylpiperazineHCID 27738751-Benzofuran-5-carbaldehydeHCID 178418339Butyllithium2 回

生成物 1

HCID 866168342-(Tributylstannyl)-1-benzofuran-5-carbaldehyde収率 34%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8058Hexane溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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%)

出典と根拠

ORDレコード
ord-f045eb7bde9240b8a2c6d4b6b3a1e309
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07781591B2

反応ノート

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