反応 #4062034
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-65f3126850e54c33abb9da18c365f6a8表示可能な構造データがありません
COC(=O)C(C(C(=O)OC)(F)F)(F)F製品情報
dimethyl 2,2,3,3-tetrafluorobutanedioate (CAS 356-36-5) 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 2737124
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
10 反応 · 10 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-65f3126850e54c33abb9da18c365f6a8反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 43.6 g (0.20 mol) of dimethyl tetrafluorosuccinate, 16.1 g (0.20 mol) of 2-chloroethanol, and 100 mL of DMSO was stirred and maintained at 25°-35° while 9.6 g (0.20 mol) of 50% NaH in mineral oil were added portionwise. The resulting mixture was stirred overnight, and then poured into 500 mL of cold water. Ether (300 mL) was added, and the resulting mixture was shaken. After mixture separated into layers, the ether layer was separated, washed with 100 mL of water, dried over CaSO4, filtered and distilled to give 23.1 g (44%) of 2-methoxy-2-(2-methoxycarbonyltetrafluoroethyl)1,3-dioxolane, b.p. 72°-72.5° at 13 Pa (0.1 mm). IR (neat) and NMR (CCl4) spectra of the product were consistent with the assigned structure. Anal.: Calcd for C8H10F4O5 :C, 36.65; H, 3.85; F, 28.99. Found: C, 36.45; H, 3.95; F, 28.70. were added portionwise The resulting mixture was stirred overnight the resulting mixture was shaken After mixture separated into layers the ether layer was separated washed with 100 mL of water dried over CaSO4 filtered distilled
ソース ID: ord-17efde729a504172899a9c4e4775a4be反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 43.6 g (0.20 mol) of dimethyl tetrafluorosuccinate, 16.1 g (0.20 mol) of 2-chloroethanol, and 100 mL of DMSO was stirred and maintained at 25°-35° while 9.6 g (0.20 mol) of 50% NaH in mineral oil were added portionwise. The resulting mixture was stirred overnight, and then poured into 500 mL of cold water. Ether (300 mL) was added, and the resulting mixture was shaken. After mixture separated into layers, the ether layer was separated, washed with 100 mL of water, dried over CaSO4, filtered and distilled to give 23.1 g (44%) of 2-methoxy-2-(2-methoxycarbonyltetrafluoroethyl)-1,3-dioxolane, b.p. 72°-72.5° at 13 Pa (0.1 mm). IR (neat) and NMR (CCl4) spectra of the product were consistent with the assigned structure. Anal.: Calcd for C8H10F4O5 : C, 36.65; H, 3.85; F, 28.99. Found: C, 36.45; H, 3.95; F, 28.70. were added portionwise The resulting mixture was stirred overnight the resulting mixture was shaken After mixture separated into layers the ether layer was separated washed with 100 mL of water dried over CaSO4 filtered distilled
ソース ID: ord-3607bd28625241678fc8f6142c3f7e2e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 43.6 g (0.20 mol) of dimethyl tetrafluorosuccinate, 16.1 g (0.20 mol) of 2-chloroethanol, and 100 mL of DMSO was stirred and maintained at 25°-35° while 9.6 g (0.20 mol) of 50% NaH in mineral oil were added portionwise. The resulting mixture was stirred overnight, and then poured into 500 mL of cold water. Ether (300 mL) was added, and the resulting mixture was shaken. After mixture separated into layers, the ether layer was separated, washed with 100 mL of water, dried over CaSO4, filtered and distilled to give 23.1 g (44%) of 2-methoxy-2-(2-methoxycarbonyltetrafluoroethyl)-1,3-dioxolane, b.p. 72°-72.5° at 13 Pa (0.1 mm). IR (neat) and NMR (CCl4) spectra of the product were consistent with the assigned structure. Anal.: Calcd. for C8H10F4O5 : C, 36.65; H, 3.85; F, 28.99. Found: C, 36.45; H, 3.95; F, 28.70. were added portionwise The resulting mixture was stirred overnight the resulting mixture was shaken After mixture separated into layers the ether layer was separated washed with 100 mL of water dried over CaSO4 filtered distilled
ソース ID: ord-51d11ba889f641ab9f1ce7f7f6fefa6f反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 43.6 g (0.20 mol) of dimethyl tetrafluorosuccinate, 16.1 g (0.20 mol) of 2-chloroethanol, and 100 mL of DMSO was stirred and maintained at 25°-35° while 9.6 g (0.20 mol) of 50% NaH in mineral oil were added portionwise. The resulting mixture was stirred overnight, and then poured into 500 mL of cold water. Ether (300 mL) was added, and the resulting mixture was shaken. After mixture separated into layers, the ether layer was separated, washed with 100 mL of water, dried over CaSO4, filtered and distilled to give 23.1 g (44%) of 2-methoxy-2-(2-methoxycarbonyltetrafluoroethyl)1,3-dioxolane, b.p. 72°-72.5° at 13 Pa (0.1 mm). IR (neat) and NMR (CCl4) spectra of the product were consistent with the assigned structure. Anal.: Calcd for C8H10F4O5 :C, 36.65; H, 3.85; F, 28.99. Found: C, 36.45; H, 3.95; F, 28.70. were added portionwise The resulting mixture was stirred overnight the resulting mixture was shaken After mixture separated into layers the ether layer was separated washed with 100 mL of water dried over CaSO4 filtered distilled
ソース ID: ord-17efde729a504172899a9c4e4775a4be反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-65f3126850e54c33abb9da18c365f6a8反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 43.6 g (0.20 mol) of dimethyl tetrafluorosuccinate, 16.1 g (0.20 mol) of 2-chloroethanol, and 100 mL of DMSO was stirred and maintained at 25°-35° while 9.6 g (0.20 mol) of 50% NaH in mineral oil were added portionwise. The resulting mixture was stirred overnight, and then poured into 500 mL of cold water. Ether (300 mL) was added, and the resulting mixture was shaken. After mixture separated into layers, the ether layer was separated, washed with 100 mL of water, dried over CaSO4, filtered and distilled to give 23.1 g (44%) of 2-methoxy-2-(2-methoxycarbonyltetrafluoroethyl)-1,3-dioxolane, b.p. 72°-72.5° at 13 Pa (0.1 mm). IR (neat) and NMR (CCl4) spectra of the product were consistent with the assigned structure. were added portionwise The resulting mixture was stirred overnight the resulting mixture was shaken After mixture separated into layers the ether layer was separated washed with 100 mL of water dried over CaSO4 filtered distilled
ソース ID: ord-0a1296af96d040a194284b7d96aa55a7反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 43.6 g (0.20 mol) of dimethyl tetrafluorosuccinate, 16.1 g (0.20 mol) of 2-chloroethanol, and 100 mL of DMSO was stirred and maintained at 25°-35° while 9.6 g (0.20 mol) of 50% NaH in mineral oil were added portionwise. The resulting mixture was stirred overnight, and then poured into 500 mL of cold water. Ether (300 mL) was added, and the resulting mixture was shaken. After mixture separated into layers, the ether layer was separated, washed with 100 mL of water, dried over CaSO4, filtered and distilled to give 23.1 g (44%) of 2-methoxy-2-(2-methoxycarbonyltetrafluoroethyl)-1,3-dioxolane, b.p. 72°-72.5° at 13 Pa (0.1 mm). IR (neat) and NMR (CCl4) spectra of the product were consistent with the assigned structure. Anal.: Calcd for C8H10F4O5 : C, 36.65; H, 3.85; F, 28.99. Found: C, 36.45; H, 3.95; F, 28.70. were added portionwise The resulting mixture was stirred overnight the resulting mixture was shaken After mixture separated into layers the ether layer was separated washed with 100 mL of water dried over CaSO4 filtered distilled
ソース ID: ord-3607bd28625241678fc8f6142c3f7e2e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 43.6 g (0.20 mol) of dimethyl tetrafluorosuccinate, 16.1 g (0.20 mol) of 2-chloroethanol, and 100 mL of DMSO was stirred and maintained at 25°-35° while 9.6 g (0.20 mol) of 50% NaH in mineral oil were added portionwise. The resulting mixture was stirred overnight, and then poured into 500 mL of cold water. Ether (300 mL) was added, and the resulting mixture was shaken. After mixture separated into layers, the ether layer was separated, washed with 100 mL of water, dried over CaSO4, filtered and distilled to give 23.1 g (44%) of 2-methoxy-2-(2-methoxycarbonyltetrafluoroethyl)-1,3-dioxolane, b.p. 72°-72.5° at 13 Pa (0.1 mm). IR (neat) and NMR (CCl4) spectra of the product were consistent with the assigned structure. Anal.: Calcd. for C8H10F4O5 : C, 36.65; H, 3.85; F, 28.99. Found: C, 36.45; H, 3.95; F, 28.70. were added portionwise The resulting mixture was stirred overnight the resulting mixture was shaken After mixture separated into layers the ether layer was separated washed with 100 mL of water dried over CaSO4 filtered distilled
ソース ID: ord-51d11ba889f641ab9f1ce7f7f6fefa6f反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of 43.6 g (0.20 mol) of dimethyl tetrafluorosuccinate, 16.1 g (0.20 mol) of 2-chloroethanol, and 100 mL of DMSO was stirred and maintained at 25°-35° while 9.6 g (0.20 mol) of 50% NaH in mineral oil were added portionwise. The resulting mixture was stirred overnight, and then poured into 500 mL of cold water. Ether (300 mL) was added, and the resulting mixture was shaken. After mixture separated into layers, the ether layer was separated, washed with 100 mL of water, dried over CaSO4, filtered and distilled to give 23.1 g (44%) of 2-methoxy-2-(2-methoxycarbonyltetrafluoroethyl)1,3-dioxolane, b.p. 72°-72.5° at 13 Pa (0.1 mm). IR (neat) and NMR (CCl4) spectra of the product were consistent with the assigned structure. Anal.: Calcd for C8H10F4O5 :C, 36.65; H, 3.85; F, 28.99. Found: C, 36.45; H, 3.95; F, 28.70. were added portionwise The resulting mixture was stirred overnight the resulting mixture was shaken After mixture separated into layers the ether layer was separated washed with 100 mL of water dried over CaSO4 filtered distilled
ソース ID: ord-17efde729a504172899a9c4e4775a4bePubChem References
化合物の公開データベース記録に掲載された情報源です。
見積依頼
仕様、数量、納入先、用途をご連絡ください。供給可否を確認します。
