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3,4-Difluorobenzoyl chloride → 3,4-Difluorophenyl 2-[4-[2-(1-Pyrrolidinyl)ethoxy]phenyl]benzo[b]thiophen-3-yl Ketone

HRID 1387041
ノート
印刷プレビュー

反応式

HRID 1387041 の反応式
[N:1]1([CH2:6][CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([C:15]3[S:19][C:18]4[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=4[CH:16]=3)=[CH:11][CH:10]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.[F:24][C:25]1[CH:26]=[C:27]([CH:31]=[CH:32][C:33]=1[F:34])[C:28](Cl)=[O:29]>Cl[Ti](Cl)(Cl)Cl>[N:1]1([CH2:6][CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([C:15]3[S:19][C:18]4[CH:20]=[CH:21][CH:22]=[CH:23][C:17]=4[C:16]=3[C:28]([C:27]3[CH:31]=[CH:32][C:33]([F:34])=[C:25]([F:24])[CH:26]=3)=[O:29])=[CH:11][CH:10]=2)[CH2:5][CH2:4][CH2:3][CH2:2]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

4

反応物 2

HCID 27245193,4-Difluorobenzoyl chlorideHCID 106637082-[4-[2-(1-Pyrrolidinyl)ethoxy)phenyl]benzo[b]thiophene

生成物 1

HCID 211827863,4-Difluorophenyl 2-[4-[2-(1-Pyrrolidinyl)ethoxy]phenyl]benzo[b]thiophen-3-yl Ketone収率 37%

試薬・触媒・溶媒 1

HCID 24193Titanium Tetrachloride触媒

反応条件

温度
0 °C

実験手順

A slurry of 3.23 g (10 mmol) of 2-[4-[2-(1-pyrrolidinyl)ethoxy)phenyl]benzo[b]thiophene in 50 mL of 1,2′dichloroethane was treated with 1.76 g (10 mmol) of 3,4-difluorobenzoyl chloride at 0° C. The mixture was protected from light and 4.4 mL (40 mmol) TiCl4 was added dropwise. The reaction was stirred at 0° C. for 5 h at which time it was quenched by carefully pouring it into 400 mL of saturated aqueous NaHCO3. To this was added EtOAc (200 mL), and the two layers were separated. The aqueous layer was extracted with EtOAc (2×50 mL). The combined organic layers were dried over Na2SO4 and evaporated in vacuo to give a crude oil which was purified by chromatography (SiO2; 2% MeOH in CHCl3) to afford 1.7 g (3.7 mmol; 37%) of the ketone as a viscous oil.

後処理

  1. additionwas added dropwise
  2. customwas quenched
  3. additionby carefully pouring it into 400 mL of saturated aqueous NaHCO3
  4. additionTo this was added EtOAc (200 mL)
  5. customthe two layers were separated
  6. extractionThe aqueous layer was extracted with EtOAc (2×50 mL)
  7. dry with materialThe combined organic layers were dried over Na2SO4
  8. customevaporated in vacuo
  9. customto give a crude oil which
  10. customwas purified by chromatography (SiO2; 2% MeOH in CHCl3)

出典と根拠

ORDレコード
ord-874355640211463283c6df3784098cdc
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06265575B1

反応ノート

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