反応 #4132006
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-99f51dea1ae14e6d972cca9949c44bad表示可能な構造データがありません
CC(C)(C)OC(=O)NN=C1CCOC1製品情報
tert-butyl N-(oxolan-3-ylideneamino)carbamate (CAS 158020-60-1) 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 72309493
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-99f51dea1ae14e6d972cca9949c44bad反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-f226e4d5d92d4fe8a3d9d17c80d2d0f3反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-a39d05a076bc40b8b4c1258d753e9bb2反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: t-butyl 2-[dihydrofuran-3(2H)-ylidene]hydrazinecarboxylate (17.26 g) was suspended in water (130 mL). Acetic acid (57.2 mL) was added to the suspension at room temperature. The mixture was stirred at room temperature for one hour. Sodium cyanoborohydride (5.36 g) was added to the solution in small portions. The mixed solution was stirred at room temperature for two hours. The reaction mixture was cooled to 0° C. The reaction mixture was neutralized by adding a 5 N aqueous sodium hydroxide solution. The mixture was extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate and then filtered. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (5% methanol/ethyl acetate). The title compound (15.3 g) was obtained. The mixed solution was stirred at room temperature for two hours The reaction mixture was cooled to 0° C The mixture was extracted with chloroform The organic layer was dried over anhydrous magnesium sulfate filtered The filtrate was concentrated under reduced pressure The residue was purified by silica gel column chromatography (5% methanol/ethyl acetate)
ソース ID: ord-fbe183f54fa246dd90f649787478c154反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 3-oxotetrahydrofuran (10.38 g) was dissolved in methanol (200 mL), and t-butyl carbazate (17.53 g) was added to the solution. The mixture was stirred at room temperature for 12 hours. The reaction mixture was concentrated to give the title compound (27.3 g). 1H-NMR (400 MHz, CDCl3) δ (ppm): 1.52 (s, 9H), 2.46 (t, J=6.9 Hz, al), 4.10 (t, J=6.9 Hz, 2H), 4.33 (s, 2H). The reaction mixture was concentrated
ソース ID: ord-23a8f39bfbf64426b5f81b0a33ecfbdb反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 3-oxotetrahydrofuran (10.38 g) was dissolved in methanol (200 mL), and t-butyl carbazate (17.53 g) was added to the solution. The mixture was stirred at room temperature for 12 hours. The reaction mixture was concentrated to give the title compound (27.3 g). 1H-NMR (400 MHz, CDCl3) δ (ppm): 1.52 (s, 9H), 2.46 (t, J=6.9 Hz, al), 4.10 (t, J=6.9 Hz, 2H), 4.33 (s, 2H). The reaction mixture was concentrated
ソース ID: ord-23a8f39bfbf64426b5f81b0a33ecfbdb反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-99f51dea1ae14e6d972cca9949c44bad反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-f226e4d5d92d4fe8a3d9d17c80d2d0f3反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-a39d05a076bc40b8b4c1258d753e9bb2反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: t-butyl 2-[dihydrofuran-3(2H)-ylidene]hydrazinecarboxylate (17.26 g) was suspended in water (130 mL). Acetic acid (57.2 mL) was added to the suspension at room temperature. The mixture was stirred at room temperature for one hour. Sodium cyanoborohydride (5.36 g) was added to the solution in small portions. The mixed solution was stirred at room temperature for two hours. The reaction mixture was cooled to 0° C. The reaction mixture was neutralized by adding a 5 N aqueous sodium hydroxide solution. The mixture was extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate and then filtered. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (5% methanol/ethyl acetate). The title compound (15.3 g) was obtained. The mixed solution was stirred at room temperature for two hours The reaction mixture was cooled to 0° C The mixture was extracted with chloroform The organic layer was dried over anhydrous magnesium sulfate filtered The filtrate was concentrated under reduced pressure The residue was purified by silica gel column chromatography (5% methanol/ethyl acetate)
ソース ID: ord-fbe183f54fa246dd90f649787478c154反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 3-oxotetrahydrofuran (10.38 g) was dissolved in methanol (200 mL), and t-butyl carbazate (17.53 g) was added to the solution. The mixture was stirred at room temperature for 12 hours. The reaction mixture was concentrated to give the title compound (27.3 g). 1H-NMR (400 MHz, CDCl3) δ (ppm): 1.52 (s, 9H), 2.46 (t, J=6.9 Hz, al), 4.10 (t, J=6.9 Hz, 2H), 4.33 (s, 2H). The reaction mixture was concentrated
ソース ID: ord-23a8f39bfbf64426b5f81b0a33ecfbdbPubChem References
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