ChemicalBook CAS DataBase List Acetyl chloride

Acetyl chloride synthesis

11synthesis methods

Product Name:Acetyl chloride
CAS Number:75-36-5
Molecular formula:C2H3ClO
Molecular Weight:78.5

The reaction was conducted in a distillation apparatus fitted with a Vigreux column, under inert gas atmosphere. Every glassware was flame-dried, or dried in the oven at 130°C overnight. Sodium acetate (1.34 g; 16.4 mmol) and tetrabutylammonium chloride (911 mg; 3.28 mmol) were dissolved in dry THF (50 mL) and left stirring for 2 hours at room temperature. Phthaloyl dichloride was added in one portion, and the mixture was heated to 85°C for 3 hours. THF (20 mL) was added, and the temperature was increased to 100°C for 30 minutes. The receiving flask collected 49.59 g of distillate, which upon NMR analysis revealed to contain Acetyl chloride. Yield: 883 mg, 11.25 mmol (68% based on sodium acetate).

32993-05-8 Synthesis

Chlorocyclopentadienylbis(triphenylphosphine)ruthenium(II)

32993-05-8
176 suppliers
$30.00/1g

506-96-7 Synthesis

506-96-7
323 suppliers
$22.40/25G

Ruthenium, bromo(η5-2,4-cyclopentadien-1-yl)bis(triphenylphosphine)-

32993-06-9
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75-36-5
590 suppliers
$17.92/100G

Yield:32993-06-9 100% ，75-36-5 100%

Reaction Conditions:

in benzene-d6 at 20; for 9 h;Glovebox;

Steps:

Preparative Scale Ligand Exchange Reactions

General procedure: Into a dry Pyrex NMR tube were added a solution of CpRu(Cl)(PPh₃)₂(1, 0.010 mmol, 500 mL/20 mM in benzene-d₆), a solution of S=P(C₆H₄OMe-p)₃ (0.0050 mmol, 50 mL/100 mM in benzene-d₆), and benzene-d₆ (180 mL). After the sensitivity of 1 to the internal standard was measured by ³¹P NMR spectroscopy, a solution of MeC(O)Br (2, 0.020 mmol, 20 mL/1.0 M in benzene-d₆) was added and the reaction was monitored by ³¹P NMR spectroscopy. The gradual conversion of 1 to 3 was confirmed. The reaction time and yield are as follows: 0.5 h, 6.3%; 1 h, 15%; 2 h, 38%; 3 h, 62%; 4 h, 80%; 5 h, 90%; 6 h, 95%; 7 h, 98%; 8 h, 99%; 9 h, 100%.

References:

Kuniyasu, Hitoshi;Sanagawa, Atsushi;Nakajima, Takuya;Iwasaki, Takanori;Kambe, Nobuaki;Bobuatong, Karan;Ehara, Masahiro [Journal of Organometallic Chemistry,2014,vol. 769,p. 34 - 37] Location in patent:supporting information

64-19-7 Synthesis