反応 #3868496
関連文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-8b1e1e3b1d8d4fd092ea980641d422b1表示可能な構造データがありません
C1=CC=C(C(=C1)CNC(=S)N)Cl製品情報
(2-chlorophenyl)methylthiourea (CAS 19380-80-4) product identity, structure identifiers and related reaction data for chemical intermediate research and sourcing review.
想定用途
専門的研究・工業用途限定
データベース ID 22400378
安全上の注意
For professional research and industrial use only. Review the supplier safety data sheet before handling.
合成データ
11 反応 · 11 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-8b1e1e3b1d8d4fd092ea980641d422b1反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 1-(2-chlorophenyl)methyl thiourea (3 g, 14.9 mmol) and propylbromide (13.5 g, 110 mmol) in acetonitrile (20 mL) was refluxed for 5 hours. The solvent was evaporated, the residue was dissolved in 200 mL of 50% water/ether and acidified with 48% hydrobromic acid solution. The two phases were separated, the aqueous layer was washed with ether and then the aqueous layer was basified with 10% sodium carbonate solution. The liberated product was extracted with diethyl ether, washed with water and brine, dried and concentrated to give 1-(2-chlorophenyl)methyl-2-propyl-2-thiopseudourea (2.82 g, 78%); mp 112°-114° C. was refluxed for 5 hours The solvent was evaporated the residue was dissolved in 200 mL of 50% water/ether The two phases were separated the aqueous layer was washed with ether The liberated product was extracted with diethyl ether washed with water and brine dried concentrated
ソース ID: ord-629220f6940f4c29a1fb10c7dd7dc1b0反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 1-(2-chlorophenyl)methyl thiourea (3 g, 14.9 mmol) and propylbromide (13.5 g, 110 mmol) in acetonitrile (20 mL) was refluxed for 5 hours. The solvent was evaporated, the residue was dissolved in 200 mL of 50% water/ether and acidified with 48% hydrobromic acid solution. The two phases were separated, the aqueous layer was washed with ether and then the aqueous layer was basified with 10% sodium carbonate solution. The liberated product was extracted with diethyl ether, washed with water and brine, dried and concentrated to give 1-(2-chlorophenyl)methyl-2-propyl-2-thiopseudourea (2.82 g, 78%); mp 112°-114° C. was refluxed for 5 hours The solvent was evaporated the residue was dissolved in 200 mL of 50% water/ether The two phases were separated the aqueous layer was washed with ether The liberated product was extracted with diethyl ether washed with water and brine dried concentrated
ソース ID: ord-629220f6940f4c29a1fb10c7dd7dc1b0反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A solution of 2-chlorobenzylamine hydrochloride (41 g, 0.23 mol) and ammonium thiocyanate (19.28 g, 0.253 mol) in water (170 mL) was heated on the steam bath for 18 hours. This mixture was concentrated in vacuo, and the residue was taken up in toluene (1 L) and azeotroped with a Dean-Stark head. The residue was triturated with wet diethyl ether to provide 27.6 g (60%) of 1-(2-chlorophenyl)methyl thiourea. The product was recrystallized from ethanol; mp 120°-122° C. This mixture was concentrated in vacuo azeotroped with a Dean-Stark head The residue was triturated with wet diethyl ether
ソース ID: ord-3953e9b7c30c4e5e8fe42d37f310e41c反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A solution of 2-chlorobenzylamine hydrochloride (41 g, 0.23 mol) and ammonium thiocyanate (19.28 g, 0.253 mol) in water (170 mL) was heated on the steam bath for 18 hours. This mixture was concentrated in vacuo, and the residue was taken up in toluene (1 L) and azeotroped with a Dean-Stark head. The residue was triturated with wet diethyl ether to provide 27.6 g (60%) of 1-(2-chlorophenyl)methyl thiourea. The product was recrystallized from ethanol; mp 120°-122° C. This mixture was concentrated in vacuo azeotroped with a Dean-Stark head The residue was triturated with wet diethyl ether
ソース ID: ord-3953e9b7c30c4e5e8fe42d37f310e41c反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 1-(2-chlorophenyl)methyl thiourea (3 g, 14.9 mmol) and propylbromide (13.5 g, 110 mmol) in acetonitrile (20 mL) was refluxed for 5 hours. The solvent was evaporated, the residue was dissolved in 200 mL of 50% water/ether and acidified with 48% hydrobromic acid solution. The two phases were separated, the aqueous layer was washed with ether and then the aqueous layer was basified with 10% sodium carbonate solution. The liberated product was extracted with diethyl ether, washed with water and brine, dried and concentrated to give 1-(2-chlorophenyl)methyl-2-propyl-2-thiopseudourea (2.82 g, 78%); mp 112°-114° C. was refluxed for 5 hours The solvent was evaporated the residue was dissolved in 200 mL of 50% water/ether The two phases were separated the aqueous layer was washed with ether The liberated product was extracted with diethyl ether washed with water and brine dried concentrated
ソース ID: ord-629220f6940f4c29a1fb10c7dd7dc1b0反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A solution of 2-chlorobenzylamine hydrochloride (41 g, 0.23 mol) and ammonium thiocyanate (19.28 g, 0.253 mol) in water (170 mL) was heated on the steam bath for 18 hours. This mixture was concentrated in vacuo, and the residue was taken up in toluene (1 L) and azeotroped with a Dean-Stark head. The residue was triturated with wet diethyl ether to provide 27.6 g (60%) of 1-(2-chlorophenyl)methyl thiourea. The product was recrystallized from ethanol; mp 120°-122° C. This mixture was concentrated in vacuo azeotroped with a Dean-Stark head The residue was triturated with wet diethyl ether
ソース ID: ord-3953e9b7c30c4e5e8fe42d37f310e41c反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 1-(2-chlorophenyl)methyl thiourea (3 g, 14.9 mmol) and propylbromide (13.5 g, 110 mmol) in acetonitrile (20 mL) was refluxed for 5 hours. The solvent was evaporated, the residue was dissolved in 200 mL of 50% water/ether and acidified with 48% hydrobromic acid solution. The two phases were separated, the aqueous layer was washed with ether and then the aqueous layer was basified with 10% sodium carbonate solution. The liberated product was extracted with diethyl ether, washed with water and brine, dried and concentrated to give 1-(2-chlorophenyl)methyl-2-propyl-2-thiopseudourea (2.82 g, 78%); mp 112°-114° C. was refluxed for 5 hours The solvent was evaporated the residue was dissolved in 200 mL of 50% water/ether The two phases were separated the aqueous layer was washed with ether The liberated product was extracted with diethyl ether washed with water and brine dried concentrated
ソース ID: ord-354a05fc5b144785ab7ce3fd07a38d06反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A solution of 2-chlorobenzylamine hydrochloride (41 g, 0.23 mol) and ammonium thiocyanate (19.28 g, 0.253 mol) in water (170 mL) was heated on the steam bath for 18 hours. This mixture was concentrated in vacuo, and the residue was taken up in toluene (1 L) and azeotroped with a Dean-Stark head. The residue was triturated with wet diethyl ether to provide 27.6 g (60%) of 1-(2-chlorophenyl)methyl thiourea. The product was recrystallized from ethanol; mp 120°-122° C. This mixture was concentrated in vacuo azeotroped with a Dean-Stark head The residue was triturated with wet diethyl ether
ソース ID: ord-dc1c1824c1c0484bac39403a48e1faa8反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 1-(2-chlorophenyl)methyl thiourea (3 g, 14.9 mmol) and propylbromide (13.5 g, 110 mmol) in acetonitrile (20 mL) was refluxed for 5 hours. The solvent was evaporated, the residue was dissolved in 200 mL of 50% water/ether and acidified with 48% hydrobromic acid solution. The two phases were separated, the aqueous layer was washed with ether and then the aqueous layer was basified with 10% sodium carbonate solution. The liberated product was extracted with diethyl ether, washed with water and brine, dried and concentrated to give 1-(2-chlorophenyl)methyl-2-propyl-2-thiopseudourea (2.82 g, 78%); mp 112°-114° C. was refluxed for 5 hours The solvent was evaporated the residue was dissolved in 200 mL of 50% water/ether The two phases were separated the aqueous layer was washed with ether The liberated product was extracted with diethyl ether washed with water and brine dried concentrated
ソース ID: ord-629220f6940f4c29a1fb10c7dd7dc1b0反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A solution of 2-chlorobenzylamine hydrochloride (41 g, 0.23 mol) and ammonium thiocyanate (19.28 g, 0.253 mol) in water (170 mL) was heated on the steam bath for 18 hours. This mixture was concentrated in vacuo, and the residue was taken up in toluene (1 L) and azeotroped with a Dean-Stark head. The residue was triturated with wet diethyl ether to provide 27.6 g (60%) of 1-(2-chlorophenyl)methyl thiourea. The product was recrystallized from ethanol; mp 120°-122° C. This mixture was concentrated in vacuo azeotroped with a Dean-Stark head The residue was triturated with wet diethyl ether
ソース ID: ord-3953e9b7c30c4e5e8fe42d37f310e41cPubChem References
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