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Tetrahydrofuran → HCID 16103459、化合物

HRID 1513842
ノート
印刷プレビュー

反応式

HRID 1513842 の反応式
Br[C:2]1[S:6][C:5]2[C:7]([Br:11])=[C:8](Br)[S:9][C:4]=2[C:3]=1[Br:12].[C:13]1([Li])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C([O:24][CH2:25][CH2:26][CH2:27][CH3:28])CCC.[C:29](Cl)(=[O:40])[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39].[CH2:42]1COCC1>>[Br:12][C:3]1[C:4]2[S:9][C:8]([C:25](=[O:24])[CH2:26][CH2:27][CH2:28][CH2:42][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:13])=[C:7]([Br:11])[C:5]=2[S:6][C:2]=1[C:29](=[O:40])[CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH3:39]
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 5

HCID 8028TetrahydrofuranHCID 8909Butyl etherHCID 87287Undecanoyl chlorideHCID 27625682,3,5,6-Tetrabromothieno[3,2-b]thiopheneHCID 178506676HCID 178506676、化合物

生成物 1

HCID 16103459HCID 16103459、化合物収率 41.3%

反応条件

温度
-78 °C

実験手順

Di-acylation (Step A) A suspension of (2,3,5,6-tetrabromothieno[3,2,b]thiophene (10 g, 21.9 mmol) in anhydrous THF (200 mL) was cooled to −78° C. Phenyl lithium solution in n-butyl ether (1.8 mol/L, 25 mL, 45 mmol) was added dropwise and the reaction mixture was stirred at −78° C. for 4 h. Undecanoyl chloride (9.2 g, 44.9 mmol) was added to the reaction mixture via syringe while maintaining the temperature of the mixture as close to −78° C. as possible. The reaction was allowed to warm to RT over about three hours and then stirred overnight at RT. The reaction mixture was then quenched by the addition of crushed ice (200 g). The reaction mixture was stirred while the ice was allowed to melt. Most (greater than about 90%) of the THF was then removed under reduced pressure and the solid was filtered from the residual solution. The solid was suspended in water (100 mL) and stirred for 1 hr then filtered. The solid was resuspended in methanol (100 mL), stirred for 1 hr then filtered to give the product 1-{3,6-dibromo-5-undecanoylthieno[3,2-b]thiophen-2-yl}undecan-1-one as a white solid (5.75 g, 41.3% yield). 1H NMR (CD2Cl2) δ 0.90 (6H, t, J=6.3 Hz), 1.20-1.48 (28H, m), 1.68-1.73 (4H, m), and 3.11 (4H, t, J=7.2 Hz).

後処理

  1. temperaturewhile maintaining the temperature of the mixture
  2. customas close to −78° C. as possible
  3. temperatureto warm to RT over about three hours
  4. stirringstirred overnight at RT
  5. customThe reaction mixture was then quenched by the addition of crushed ice (200 g)
  6. stirringThe reaction mixture was stirred while the ice
  7. customMost (greater than about 90%) of the THF was then removed under reduced pressure
  8. filtrationthe solid was filtered from the residual solution
  9. stirringstirred for 1 hr
  10. filtrationthen filtered
  11. stirringstirred for 1 hr
  12. filtrationthen filtered

出典と根拠

ORDレコード
ord-a23fbabe24ba411c978c9f70056fc197
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217183B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート