Acetic Anhydride → Ethyl ethoxymethylene-3-oxo-4,4,4-trifluorobutyrate

反応式

[CH2:1]([O:3][C:4](=[O:12])[CH2:5][C:6](=[O:11])[C:7]([F:10])([F:9])[F:8])[CH3:2].[C:13]([O:16][C:17](=O)C)(=O)[CH3:14].C(OCC)(OCC)OCC>>[CH2:1]([O:3][C:4](=[O:12])/[C:5](=[CH:17]/[O:16][CH2:13][CH3:14])/[C:6](=[O:11])[C:7]([F:10])([F:8])[F:9])[CH3:2]

参加物

反応物 3

HCID 7918Acetic Anhydride

HCID 31214Ethyl orthoformate

HCID 67793Ethyl 4,4,4-trifluoroacetoacetate

生成物 1

HCID 6185754Ethyl ethoxymethylene-3-oxo-4,4,4-trifluorobutyrate収率 96.4%

実験手順

4,4,4-Trifluoro-3-oxo-butyric acid ethyl ester (16 g, 86.4 mmol) was dissolved in acetic anhydride (33.6 g, 329.6 mmol) and triethyl orthoformate (38.4 g, 260 mmol) was added to the mixture. The resultant mixture was refluxed for 18 hours. The mixture was concentrated under reduced pressure to obtain 20 g of 2-[1-Ethoxy-meth-(E)-ylidene]-4,4,4-trifluoro-3-oxo-butyric acid ethyl ester as crude.

後処理

concentrationThe mixture was concentrated under reduced pressure

出典と根拠

ORDレコード: ord-c69bb7231c8f41809dd60e5b3613124d
出典データセット: uspto-grants-2015_10
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09163021B2

反応ノート

読み込み中…