21009-57-4|Morpholine-3-thione| Ambeed

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CAS No. :	21009-57-4
Formula :	C₄H₇NOS
M.W :	117.17
SMILES Code :	S=C1NCCOC1

Yield	Reaction Conditions	Operation in experiment
72.2%	With Lawessons reagent; In tetrahydrofuran; for 1.5h;Heating / reflux;	Step 2: MorPholin-3-thione; A mixture of <strong>[109-11-5]morpholin-3-one</strong> (4.7 g) and Lawesson's reagent (10.3 g) in dry THF (94 mL) was heated to reflux for 1.5 h. The reaction mixture was cooled to room temperature and the reaction solvent was removed in vacuo. The residue was applied to silica gel column chromatography and eluted with CHCI3-methanol (50 : 1) to obtain a yellow solid. Recrystallization of the crude product from hexane-ethyl acetate gave the title (4.0 g, 72.2%) as yellow powder. 1H NMR (CDCI3) 8 3.45 (t, 2H, J = 5.1 Hz), 3.91 (t, 2H, J = 5.1 Hz), 4.55 (s, 2H).
72.2%	With Lawessons reagent; In tetrahydrofuran; for 1.5h;Heating / reflux;	A mixture of <strong>[109-11-5]morpholin-3-one</strong> (4.7 g) and Lawesson's reagent (10.3 g) in dry THF (94 mL) was36USlDOCS 5763327vl EPO <DP n="38"/>heated to reflux for 1.5 h. The reaction mixture was cooled to room temperature and the reaction solvent was removed in vacuo. The residue was applied to silica gel column chromatography and eluted with CHCI3: methanol (50:1) to obtain a yellow solid. Recrystallization of the crude product from hexane:ethyl acetate gave the title compound (4.0 g, 72.2%) as a yellow powder. 1H NMR (CDCI3) δ 3.45 (t, 2H, J= 5.1 Hz), 3.91 (t, 2H, J = 5.1 Hz), 4.55 (s, 2H).
72.2%	With Lawessons reagent; In tetrahydrofuran; for 1.5h;Heating / reflux;	Step 2: Morpholin-3-thione A mixture of <strong>[109-11-5]morpholin-3-one</strong> (4.7 g) and Lawesson's reagent (10.3 g) in dry THF (94 mL) was heated to reflux for 1.5 h. The reaction mixture was cooled to room temperature and the reaction solvent was removed in vacuo. The residue was applied to silica gel column chromatography and eluted with CHCI3-methanol (50: 1) to obtain a yellow solid. Recrystallization of the crude product from hexane-ethyl acetate gave the title (4.0 g, 72.2%) as yellow powder. 'H NMR (CDCI3) 8 3.45 (t, 2H, J = 5.1 Hz), 3.91 (t, 2H, J = 5.1 Hz), 4.55 (s, 2H).

72.2%	With Lawessons reagent; In tetrahydrofuran; for 1.5h;Heating / reflux;	A mixture of <strong>[109-11-5]morpholin-3-one</strong> (4.7 g) and Lawesson's reagent (10.3 g) in dry THF (94 mL) was heated to reflux for 1.5 h. The reaction mixture was cooled to room temperature and the reaction solvent was removed in vacuo. The residue was applied to silica gel column chromatography and eluted with CHCl3-methanol (50:1) to obtain a yellow solid. Recrystallization of the crude product from hexane-ethyl acetate gave the title (4.0 g, 72.2%) as yellow powder. 1H NMR (CDCl3) δ 3.45 (t, 2H, J=5.1 Hz), 3.91 (t, 2H, J=5.1 Hz), 4.55 (s, 2H).
47.94%	With Lawessons reagent; In tetrahydrofuran; for 16h;Reflux;	To the solution of compound 76 (1.8g, 17.82mmol, 1.0eq) in tetrahydrofuran (30mL) was added Lawesson's reagent (3.59g, 8.91mmol, 0.5eq). Reaction mixture was refluxed for 16h. After completion of reaction, reaction mixture was transferred into water and product was extracted with ethyl acetate. Organic layer was combined, washed with brine solution, dried over sodium sulfate and concentrated under reduced pressure to obtain crude material. This was further purified by column chromatography and the compound was eluted in 15% ethyl acetate in hexane to obtain 76.1. (1.0g, Yield: 47.94%). MS(ES): m/z 119.02 [M+H] +.

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CAS No.: 21009-57-4

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CAS No.: 21009-57-4

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Product Details of [ 21009-57-4 ]

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[ 21009-57-4 ] Synthesis Path-Downstream 1~1

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Physical hazards
Code	Phrase
H200	Unstable explosive
H201	Explosive; mass explosion hazard
H202	Explosive; severe projection hazard
H203	Explosive; fire, blast or projection hazard
H204	Fire or projection hazard
H205	May mass explode in fire
H220	Extremely flammable gas
H221	Flammable gas
H222	Extremely flammable aerosol
H223	Flammable aerosol
H224	Extremely flammable liquid and vapour
H225	Highly flammable liquid and vapour
H226	Flammable liquid and vapour
H227	Combustible liquid
H228	Flammable solid
H229	Pressurized container: may burst if heated
H230	May react explosively even in the absence of air
H231	May react explosively even in the absence of air at elevated pressure and/or temperature
H240	Heating may cause an explosion
H241	Heating may cause a fire or explosion
H242	Heating may cause a fire
H250	Catches fire spontaneously if exposed to air
H251	Self-heating; may catch fire
H252	Self-heating in large quantities; may catch fire
H260	In contact with water releases flammable gases which may ignite spontaneously
H261	In contact with water releases flammable gas
H270	May cause or intensify fire; oxidizer
H271	May cause fire or explosion; strong oxidizer
H272	May intensify fire; oxidizer
H280	Contains gas under pressure; may explode if heated
H281	Contains refrigerated gas; may cause cryogenic burns or injury
H290	May be corrosive to metals
Health hazards
Code	Phrase
H300	Fatal if swallowed
H301	Toxic if swallowed
H302	Harmful if swallowed
H303	May be harmful if swallowed