* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With indium In neat (no solvent) at 20℃; for 8 h; Inert atmosphere; Sonication
General procedure: In a flame dried Schlenk tube (fitted with a Teflon plug valve) 1.2 mmol (0.127 g) of No.15 butanoyl chloride (2a) was added to a stirred mixture of 1.0 mmol (0.402 g) of No.16 tributyl(3-chlorophenyl)stannane (1f) and No.17 indium powder (0.148 g, 1.0 mmol) under a nitrogen gas stream. After purging the system with nitrogen by means of three pump-fill cycles, the tube was capped and immersed in a water–detergent bath at 60 °C. The ultrasonic titanium horn was placed into the bath to a distance of 10 mm to the wall and 5 mm from the bottom of the Schlenk tube and ultrasound was applied in a pulsed mode (duty cycle = 70percent; output power = 70percent) for 10 min. After addition of 10percent (m/v) solution of No.18 NaOH (2 mL) and 10 μL of No.19 tetradecane (internal standard), the mixture was stirred at room temperature for 15 min and then diluted with DCM (5 mL). Once the stirring was stopped for about 5 min, the supernatant liquid mixture was decanted into a separatory funnel. The silvery-white solid, settled at the bottom of the Schlenk tube, was washed with acetone (2 × 5 mL), deionized water (2 × 5 mL), and then vacuum-dried at room temperature. As indicated by DSC analysis, the dried sample (0.133 g) meant a 90percent recovered yield of pure No.20 indium. On the other hand, the organic phase was successively washed with water and brine, dried over Na2SO4, filtered, analyzed by GC, and then concentrated in vacuo. Purification by column chromatography on silica gel (60 ?, 70–230 mesh) doped with 10percent of KF (hexanes/DCM 8:2) gave 0.096 g (53percent) of 3fa as a colorless oil.
Reference：
[1] Journal of Catalysis, 2005, vol. 230, # 2, p. 375 - 383
12
[ 6575-13-9 ]
[ 2142-76-9 ]
Reference：
[1] Synthesis, 1993, # 10, p. 985 - 992
13
[ 14765-50-5 ]
[ 2142-76-9 ]
Reference：
[1] Bulletin de la Societe Chimique de France, 1967, p. 650 - 657
14
[ 576-22-7 ]
[ 75-36-5 ]
[ 2142-76-9 ]
Reference：
[1] Tetrahedron, 1969, vol. 25, p. 4455 - 4465
[2] Tetrahedron, 1996, vol. 52, # 3, p. 861 - 868
[3] Synlett, 2005, # 14, p. 2167 - 2170
15
[ 576-22-7 ]
[ 2142-76-9 ]
Reference：
[1] Journal of Medicinal Chemistry, 2013, vol. 56, # 1, p. 84 - 96
16
[ 917-64-6 ]
[ 6575-13-9 ]
[ 2142-76-9 ]
Reference：
[1] Journal of the Chemical Society, 1956, p. 4673
[2] Organic Mass Spectrometry, 1993, vol. 28, # 10, p. 1107 - 1110
[3] Chemische Berichte, 1997, vol. 130, # 5, p. 585 - 592
17
[ 917-54-4 ]
[ 21900-37-8 ]
[ 2142-76-9 ]
Reference：
[1] Journal of Organic Chemistry, 1980, vol. 45, # 19, p. 3892 - 3902
18
[ 82204-76-0 ]
[ 2142-76-9 ]
Reference：
[1] Synthesis, 1993, # 10, p. 985 - 992
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
1-2 Day Shipping
