ChemicalBook CAS DataBase List 2-Chloro-thiophene-5-isocyanate

2-Chloro-thiophene-5-isocyanate synthesis

2synthesis methods

Product Name:2-Chloro-thiophene-5-isocyanate
CAS Number:76537-13-8
Molecular formula:C5H2ClNOS
Molecular Weight:159.59

24065-33-6 Synthesis

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Yield:-

Reaction Conditions:

Stage #1:5-Chlorothiophene-2-carboxylic acid with Chloro-oxo-acetic acid;N,N-dimethyl-formamide in dichloromethane for 1.16667 h;
Stage #2: with sodium azide in toluene at 20;

Steps:

48.A
To a suspension of 5-chloro-2-thiophenecarboxylic acid (650 mg, 4.00 mmol) in CH₂Cl₂ (8 mL) containing 3 drops of DMF, oxalyl chloride (0.700 mL, 8.00 mmol) was added. The suspension became clear after 10 min of stirring. After being stirred for 1 h, the mixture was concentrated in vacuo. The residue was dissolved in toluene (8 mL). NaN₃ (540 mg, 8.31 mmol) was added. The mixture was stirred at room temperature overnight. It was EPO then filtered. The filtrate was heated at 100 ⁰C for 3 h. The solution was filtered, and used in the next reaction.

References:

PORTOLA PHARMACEUTICALS, INC. WO2006/55951, 2006, A2 Location in patent:Page/Page column 68-69

Ethanamine, N-[(3,5-dichlorophenyl)methylene]-2,2-diethoxy-

1000210-73-0
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76537-13-8
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$165.00/250mg

References