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Dimethylformamide → Tetradecyl-2-formylthiophene-3-carboxylate

HRID 523439
ノート
印刷プレビュー

反応式

HRID 523439 の反応式
C(NC(C)C)(C)C.C([Li])CCC.[CH2:13]([O:27][C:28]([C:30]1[CH:34]=[CH:33][S:32][CH:31]=1)=[O:29])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26].CN([CH:38]=[O:39])C>CCCCCC.C1COCC1.C(OCC)C.C(O)(=O)C>[CH2:13]([O:27][C:28]([C:30]1[CH:34]=[CH:33][S:32][C:31]=1[CH:38]=[O:39])=[O:29])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]
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

9

反応物 4

HCID 6228DimethylformamideHCID 7912DiisopropylamineHCID 86717683Tetradecylthiophene-3-carboxylateHCID 178418339Butyllithium

生成物 1

HCID 86717684Tetradecyl-2-formylthiophene-3-carboxylate

試薬・触媒・溶媒 4

HCID 176Acetic Acid溶媒
HCID 3283
Diethyl Ether
溶媒
HCID 8028Tetrahydrofuran溶媒2 回
HCID 8058Hexane溶媒

反応条件

温度
-78 °C

実験手順

To a 100 mL Schlenk flask were added 0.5 mL of diisopropyl amine and 20 mL of dry THF. The flask was cooled to −78° C. 3.5 mmol of n-butyl lithium in hexane was then added to the above solution. The mixture was stirred at −78° C. for 30 minutes. After stirring, 1.0 g of tetradecylthiophene-3-carboxylate in 10 mL THF was added dropwise to the solution. After stirring at −78° C. for another 2 hours, 0.7 mL of DMF was syringed into the reaction mixture. The reaction mixture was stirred for 5 h at −78° C. and 1 mL of acetic acid was added to the flask. The mixture was poured into a separation funnel and diethyl ether was added to the mixture. The organic layer was washed 3 times with 100 mL of water, dried with MgSO4, and the solvents were removed by rotary evaporation. The resulting residue was purified by column chromatography using a mixture of hexane and dichloromethane to give the desired compound. The NMR data were obtained and were consistent with those of the desired compound.

後処理

  1. stirringAfter stirring
  2. stirringAfter stirring at −78° C. for another 2 hours
  3. stirringThe reaction mixture was stirred for 5 h at −78° C.
  4. additionThe mixture was poured into a separation funnel
  5. washThe organic layer was washed 3 times with 100 mL of water
  6. dry with materialdried with MgSO4
  7. customthe solvents were removed by rotary evaporation
  8. customThe resulting residue was purified by column chromatography
  9. additiona mixture of hexane and dichloromethane

出典と根拠

ORDレコード
ord-fa7559aed06e47e5b98fcfcb0b1791e9
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09337358B2

反応ノート

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