反応 #3854883
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-871712ba7aa341548fa5a1834b51a263表示可能な構造データがありません
CC(C)OC(=O)C1=CC(=CC=C1)N製品情報
propan-2-yl 3-aminobenzoate (CAS 35005-25-5) 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 236743
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
7 反応 · 7 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-871712ba7aa341548fa5a1834b51a263反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Thionyl chloride (3.5 g, 0.029 mole) was added to a stirred mixture of 5,6-dihydro-2-methyl-1,4-oxathiin-3-carboxylic acid (4.7 g, 0.029 mole) and methylene chloride (100 ml). The mixture was warmed to 30°-35° C. for 4 hours, then evaporated under reduced pressure. The residue, crude 5,6-dihydro-2-methyl-1,4-oxathiin-3-carbonyl chloride, was dissolved in methylene chloride (100 ml), and the ice-chilled solution treated dropwise with a solution of 1-methylethyl 3-aminobenzoate (5,.2 g, 0.029 mole) and triethylamine (2.9 g, 0.029 mole) in methylene chloride (50 ml). The reaction mixture was stirred overnight at room temperature and then worked up by washing in sequence with water, dilute hydrochloric acid, water, 2% sodium hydroxide and water. Evaporation of the solvent left an oil, which solidified. After recrystallization from ethanol (30 ml) the product (4.0 g, 42% yield) melted at 92°-94° C. Analysis: Calc.: C 59.79, H 5.96, N 4.36, Found: C 59.46, H 6.21, N 4.51 The mixture was warmed to 30°-35° C. for 4 hours evaporated under reduced pressure The residue, crude 5,6-dihydro-2-methyl-1,4-oxathiin-3-carbonyl chloride, was dissolved in methylene chloride (100 ml) the ice-chilled solution by washing in sequence with water, dilute hydrochloric acid, water, 2% sodium hydroxide and water Evaporation of the solvent left an oil, which
ソース ID: ord-5ea1d1f5095d41dea5f98b013b7502e1反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Thionyl chloride (3.5 g, 0.029 mole) was added to a stirred mixture of 5,6-dihydro-2-methyl-1,4-oxathiin-3-carboxylic acid (4.7 g, 0.029 mole) and methylene chloride (100 ml). The mixture was warmed to 30°-35° C. for 4 hours, then evaporated under reduced pressure. The residue, crude 5,6-dihydro-2-methyl-1,4-oxathiin-3-carbonyl chloride, was dissolved in methylene chloride (100 ml), and the ice-chilled solution treated dropwise with a solution of 1-methylethyl 3-aminobenzoate (5,.2 g, 0.029 mole) and triethylamine (2.9 g, 0.029 mole) in methylene chloride (50 ml). The reaction mixture was stirred overnight at room temperature and then worked up by washing in sequence with water, dilute hydrochloric acid, water, 2% sodium hydroxide and water. Evaporation of the solvent left an oil, which solidified. After recrystallization from ethanol (30 ml) the product (4.0 g, 42% yield) melted at 92°-94° C. Analysis: Calc.: C 59.79, H 5.96, N 4.36, Found: C 59.46, H 6.21, N 4.51 The mixture was warmed to 30°-35° C. for 4 hours evaporated under reduced pressure The residue, crude 5,6-dihydro-2-methyl-1,4-oxathiin-3-carbonyl chloride, was dissolved in methylene chloride (100 ml) the ice-chilled solution by washing in sequence with water, dilute hydrochloric acid, water, 2% sodium hydroxide and water Evaporation of the solvent left an oil, which
ソース ID: ord-5ea1d1f5095d41dea5f98b013b7502e1反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Thionyl chloride (3.5 g, 0.029 mole) was added to a stirred mixture of 5,6-dihydro-2-methyl-1,4-oxathiin-3-carboxylic acid (4.7 g, 0.029 mole) and methylene chloride (100 ml). The mixture was warmed to 30°-35° C. for 4 hours, then evaporated under reduced pressure. The residue, crude 5,6-dihydro-2-methyl-1,4-oxathiin-3-carbonyl chloride, was dissolved in methylene chloride (100 ml), and the ice-chilled solution treated dropwise with a solution of 1-methylethyl 3-aminobenzoate (5,.2 g, 0.029 mole) and triethylamine (2.9 g, 0.029 mole) in methylene chloride (50 ml). The reaction mixture was stirred overnight at room temperature and then worked up by washing in sequence with water, dilute hydrochloric acid, water, 2% sodium hydroxide and water. Evaporation of the solvent left an oil, which solidified. After recrystallization from ethanol (30 ml) the product (4.0 g, 42% yield) melted at 92°-94° C. Analysis: Calc.: C 59.79, H 5.96, N 4.36, Found: C 59.46, H 6.21, N 4.51 The mixture was warmed to 30°-35° C. for 4 hours evaporated under reduced pressure The residue, crude 5,6-dihydro-2-methyl-1,4-oxathiin-3-carbonyl chloride, was dissolved in methylene chloride (100 ml) the ice-chilled solution by washing in sequence with water, dilute hydrochloric acid, water, 2% sodium hydroxide and water Evaporation of the solvent left an oil, which
ソース ID: ord-5ea1d1f5095d41dea5f98b013b7502e1反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-871712ba7aa341548fa5a1834b51a263反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Thionyl chloride (3.5 g, 0.029 mole) was added to a stirred mixture of 5,6-dihydro-2-methyl-1,4-oxathiin-3-carboxylic acid (4.7 g, 0.029 mole) and methylene chloride (100 ml). The mixture was warmed to 30°-35° C. for 4 hours, then evaporated under reduced pressure. The residue, crude 5,6-dihydro-2-methyl-1,4-oxathiin-3-carbonyl chloride, was dissolved in methylene chloride (100 ml), and the ice-chilled solution treated dropwise with a solution of 1-methylethyl 3-aminobenzoate (5,.2 g, 0.029 mole) and triethylamine (2.9 g, 0.029 mole) in methylene chloride (50 ml). The reaction mixture was stirred overnight at room temperature and then worked up by washing in sequence with water, dilute hydrochloric acid, water, 2% sodium hydroxide and water. Evaporation of the solvent left an oil, which solidified. After recrystallization from ethanol (30 ml) the product (4.0 g, 42% yield) melted at 92°-94° C. The mixture was warmed to 30°-35° C. for 4 hours evaporated under reduced pressure The residue, crude 5,6-dihydro-2-methyl-1,4-oxathiin-3-carbonyl chloride, was dissolved in methylene chloride (100 ml) the ice-chilled solution by washing in sequence with water, dilute hydrochloric acid, water, 2% sodium hydroxide and water Evaporation of the solvent left an oil, which
ソース ID: ord-90e45774744b44b68e872e5d0e88e619反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Thionyl chloride (3.5 g, 0.029 mole) was added to a stirred mixture of 5,6-dihydro-2-methyl-1,4-oxathiin-3-carboxylic acid (4.7 g, 0.029 mole) and methylene chloride (100 ml). The mixture was warmed to 30°-35° C. for 4 hours, then evaporated under reduced pressure. The residue, crude 5,6-dihydro-2-methyl-1,4-oxathiin-3-carbonyl chloride, was dissolved in methylene chloride (100 ml), and the ice-chilled solution treated dropwise with a solution of 1-methylethyl 3-aminobenzoate (5,.2 g, 0.029 mole) and triethylamine (2.9 g, 0.029 mole) in methylene chloride (50 ml). The reaction mixture was stirred overnight at room temperature and then worked up by washing in sequence with water, dilute hydrochloric acid, water, 2% sodium hydroxide and water. Evaporation of the solvent left an oil, which solidified. After recrystallization from ethanol (30 ml) the product (4.0 g, 42% yield) melted at 92°-94° C. Analysis: Calc.: C 59.79, H 5.96, N 4.36, Found: C 59.46, H 6.21, N 4.51 The mixture was warmed to 30°-35° C. for 4 hours evaporated under reduced pressure The residue, crude 5,6-dihydro-2-methyl-1,4-oxathiin-3-carbonyl chloride, was dissolved in methylene chloride (100 ml) the ice-chilled solution by washing in sequence with water, dilute hydrochloric acid, water, 2% sodium hydroxide and water Evaporation of the solvent left an oil, which
ソース ID: ord-5ea1d1f5095d41dea5f98b013b7502e1PubChem References
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