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Methyl 3-hydroxy-4-((triMethylsilyl)ethynyl)benzoate

Product Name
Methyl 3-hydroxy-4-((triMethylsilyl)ethynyl)benzoate
CAS No.
478169-68-5
Chemical Name
Methyl 3-hydroxy-4-((triMethylsilyl)ethynyl)benzoate
Synonyms
Lifitegrast Impurity 94;Propanoicacid,6-methoxy-;Methyl 3-hydroxy-4-((triMethylsilyl)ethynyl)benzoate;methyl 3-hydroxy-4-(2-(trimethylsilyl)ethynyl)benzoate;Methyl 3-hydroxy-4-((trimethylsilyl)ethynyl)benzoate - [M56992];Benzoic acid, 3-hydroxy-4-[2-(trimethylsilyl)ethynyl]-, methyl ester
CBNumber
CB32735811
Molecular Formula
C13H16O3Si
Formula Weight
248.35
MOL File
478169-68-5.mol
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Methyl 3-hydroxy-4-((triMethylsilyl)ethynyl)benzoate Property

Boiling point:
332.2±42.0 °C(Predicted)
Density 
1.10±0.1 g/cm3(Predicted)
storage temp. 
Inert atmosphere,Room Temperature
pka
8.80±0.40(Predicted)
Appearance
Light yellow to yellow Solid
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Hazard and Precautionary Statements (GHS)

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N-Bromosuccinimide Price

Synthonix
Product number
M56992
Product name
Methyl3-hydroxy-4-((trimethylsilyl)ethynyl)benzoate
Purity
98%
Packaging
100mg
Price
$50
Updated
2021/12/16
Synthonix
Product number
M56992
Product name
Methyl3-hydroxy-4-((trimethylsilyl)ethynyl)benzoate
Purity
98%
Packaging
250mg
Price
$80
Updated
2021/12/16
Synthonix
Product number
M56992
Product name
Methyl3-hydroxy-4-((trimethylsilyl)ethynyl)benzoate
Purity
98%
Packaging
1g
Price
$190
Updated
2021/12/16
Activate Scientific
Product number
AS44936
Product name
Methyl 3-hydroxy-4-((trimethylsilyl)ethynyl)benzoate
Purity
98%
Packaging
100mg
Price
$206
Updated
2021/12/16
Activate Scientific
Product number
AS44936
Product name
Methyl 3-hydroxy-4-((trimethylsilyl)ethynyl)benzoate
Purity
98%
Packaging
250mg
Price
$390
Updated
2021/12/16
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Methyl 3-hydroxy-4-((triMethylsilyl)ethynyl)benzoate Chemical Properties,Usage,Production

Synthesis

157942-12-6

1066-54-2

478169-68-5

Methyl 3-hydroxy-4-iodobenzoate (5.22 g, 18.8 mmol) and trimethylsilylacetylene (3.71 mL, 26.3 mmol) were used as raw materials, which were added under nitrogen protection along with bis(triphenylphosphine)palladium dichloride (386 mg, 0.55 mmol) and cuprous iodide (54 mg, 0.28 mmol) in a dry THF (20 mL ) and CHCl3 (40 mL) in a solvent mixture. Subsequently, triethylamine (8.14 mL, 58.4 mmol) was added to the reaction system and the mixture was heated to 50 °C for 4 hours. After completion of the reaction, the reaction mixture was diluted with CHCl3 (60 mL), washed sequentially with 5% HCl (2 x 40 mL), and the organic phase was dried with MgSO4 and concentrated to give a brown oily solid (8.31 g). The crude product was purified by column chromatography (Biotage standard column, 90 g silica gel), eluting first with 10% EtOAc/hexane (1 L) and then with 15% EtOAc/hexane (1 L). The fraction containing the target product was collected and concentrated to give methyl 3-hydroxy-4-((trimethylsilyl)alkynyl)benzoate (4.22 g, 91% yield) as a yellow solid. High-resolution mass spectrometry (FAB) analysis results: C13H16O3Si [M+H]+ calculated value 249.0947, measured value 249.0947.

References

[1] Journal of Medicinal Chemistry, 2006, vol. 49, # 14, p. 4425 - 4436
[2] Patent: US2003/232853, 2003, A1. Location in patent: Page 38
[3] Patent: US2003/73707, 2003, A1
[4] Patent: US2003/105089, 2003, A1

Methyl 3-hydroxy-4-((triMethylsilyl)ethynyl)benzoate Preparation Products And Raw materials

Raw materials

Preparation Products

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Methyl 3-hydroxy-4-((triMethylsilyl)ethynyl)benzoate Suppliers

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478169-68-5, Methyl 3-hydroxy-4-((triMethylsilyl)ethynyl)benzoateRelated Search:


  • Methyl 3-hydroxy-4-((triMethylsilyl)ethynyl)benzoate
  • methyl 3-hydroxy-4-(2-(trimethylsilyl)ethynyl)benzoate
  • Benzoic acid, 3-hydroxy-4-[2-(trimethylsilyl)ethynyl]-, methyl ester
  • Propanoicacid,6-methoxy-
  • Methyl 3-hydroxy-4-((trimethylsilyl)ethynyl)benzoate - [M56992]
  • Lifitegrast Impurity 94
  • 478169-68-5