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[ CAS No. 89729-09-9 ]

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Chemical Structure| 89729-09-9
Chemical Structure| 89729-09-9
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Product Details of [ 89729-09-9 ]

CAS No. :89729-09-9 MDL No. :MFCD09832878
Formula : C5H8O3S Boiling Point : 242.8°C at 760 mmHg
Linear Structure Formula :- InChI Key :N/A
M.W :148.18 g/mol Pubchem ID :-
Synonyms :

Safety of [ 89729-09-9 ]

Signal Word:Warning Class:
Precautionary Statements:P261-P264-P270-P271-P280-P301+P312-P302+P352-P304+P340-P305+P351+P338-P330-P332+P313-P337+P313-P362-P403+P233-P405-P501 UN#:
Hazard Statements:H302-H315-H319-H335 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 89729-09-9 ]

  • Downstream synthetic route of [ 89729-09-9 ]

[ 89729-09-9 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 39590-81-3 ]
  • [ 89729-09-9 ]
YieldReaction ConditionsOperation in experiment
93% With thionyl chloride; In dichloromethane; at -5℃; for 2.5h; (0236) To a stirred solution of <strong>[39590-81-3](1-hydroxymethyl-cyclopropyl)-methanol</strong> (Combi-blocks, 10.0 g, 97.9 mmol) and triethylamine (22.0 g, 220 mmol) in DCM (120 mL) at -5 C. was added thionyl chloride (13.0 g, 110 mmol) dropwise over 30 min. The resulting suspension was stirred at -5 C. for an additional 2 h and then diluted with water (100 mL). The organic phase was separated, washed with brine, dried over sodium sulfate and filtered. The filtrate was dried under reduced pressure to give 5,7-dioxa-6-thia-spiro[2.5]octane 6-oxide as a white solid (13.5 g, 93%). 1HNMR (CDCl3, 300 MHz): delta 5.26-5.30 (d, 2H, J=11.4 Hz), 3.06-3.10 (d, 2H, J=11.7 Hz), 0.84-0.89 (m, 2H), 0.49-0.54 (m, 2H).
93% With thionyl chloride; triethylamine; In dichloromethane; at 0 - 20℃; 1,1-cyclopropanedimethanol (102 g, 1 Omol) was dissolved in dichloromethane,Triethylamine (303 g, 3 Omol) was added, cooled to 0 C, thionyl chloride (238 g, 2 Omol) was added dropwise, and reacted at 0 C to room temperature for 6-8 hours.The reaction was quenched by the addition of saturated ammonium chloride solution, separated, the organic phase was concentrated to remove the solvent and a small amount of petroleum ether was beaten to obtain 137.4 g of the yellow solid product 1,1_cyclopropanedimethanol sulfinate and the molar yield was 93%.
With thionyl chloride; triethylamine; In dichloromethane; at -5℃; for 8h; EXAMPLE 16: PREPARATION OF 1 ,1 -CYCLOPROPANEDIIVIETHANOL CYCLOSULFITE (FORMULA XVIII):1 ,1-cyclopropanedimethanol (23 kg) and triethyl amine (63 liters) were taken into a glass-lined reactor containing dichloromethane (575 liters). The reaction mass was cooled to about -5 0C. Thionyl chloride (17.5 liters) was added slowly at about -5 0C over about 6 hours followed by stirring for about 2 hours at about -5 0C. The reaction mass was decomposed slowly at below 15 0C by the addition of the reaction mass to a disodium hydrogen orthophosphate solution (19.5 kg of disodium hydrogen orthophosphate dissolved in 575 L of water and the pH adjusted to about 7 by the addition of 1 L of orthophosphoric acid). The organic layer was separated and the aqueous layer was extracted with dichloromethane (2*140 liters). The combined organic layer was washed with 5% NaHCO3 solution (7.5 kg dissolved in 155 L of water).The obtained organic layer was taken into a clean reactor followed by adding carbon (2.5 kg) and sodium sulfate (5.5 kg). The reaction mixture was stirred at about 30 0C for about 20 minutes. The reaction mass was filtered through a celite bed and the bed was washed with dichloromethane (25 liters). The resultant filtrate was passed through a micro filter and the solvent distilled completely at about 45 0C to afford a residue of the title compound.To the obtained residue, n-hexane (70 liters) was added followed by stirring at about 10 0C for about 1 hour. The separated solid was filtered and washed with precooled n-hexane (25 liters) to afford 23.0 kg of the title compound. EPO <DP n="37"/>Purity by GC: 92.19%.
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