Phosphorus oxide (P4O10) → Ethyl (E)-4,4,5,5-tetrafluoropent-2-enoate

反応式

[F:1][C:2]([F:14])([CH:11]([F:13])[F:12])[CH:3](O)[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>>[F:1][C:2]([F:14])([CH:11]([F:12])[F:13])/[CH:3]=[CH:4]/[C:5]([O:7][CH2:8][CH3:9])=[O:6]

参加物

反応物 2

HCID 14812Phosphorus oxide (P4O10)

HCID 86691164Ethyl 4,4,5,5-tetrafluoro-3-hydroxy-pentanoate

生成物 1

HCID 86691166Ethyl (E)-4,4,5,5-tetrafluoropent-2-enoate収率 76.2%

反応条件

温度: 80 °C

実験手順

Ethyl 4,4,5,5-tetrafluoro-3-hydroxy-pentanoate (22.9 g, 0.105 mol) was mixed with phosphorus pentoxide (7.5 g, 0.053 mol) and the resulting mixture was stirred at 80° C. for two hours. The product was isolated by vacuum distillation (53 mbar, 92° C.) to yield 15.9 g of a liquid (0.08 mol, 76%) that was used directly in the next step.

後処理

customThe product was isolated by vacuum distillation (53 mbar, 92° C.)

出典と根拠

ORDレコード: ord-0d0129ee485745a1b62bf2c8a12e4307
出典データセット: uspto-grants-2014_11
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08883791B2

反応ノート

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