4-Chloro-3-(trifluoromethyl)phenol → 4-(4-Chloro-3-trifluoromethyl-phenoxy)-3-fluoro-benzaldehyde

反応式

[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][C:3]=1[C:9]([F:12])([F:11])[F:10].[F:13][C:14]1[CH:15]=[C:16]([CH:19]=[CH:20][C:21]=1F)[CH:17]=[O:18]>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C:21]2[CH:20]=[CH:19][C:16]([CH:17]=[O:18])=[CH:15][C:14]=2[F:13])=[CH:4][C:3]=1[C:9]([F:10])([F:11])[F:12]

参加物

反応物 2

HCID 805204-Chloro-3-(trifluoromethyl)phenol

HCID 5880883,4-Difluorobenzaldehyde

生成物 1

HCID 866661984-(4-Chloro-3-trifluoromethyl-phenoxy)-3-fluoro-benzaldehyde収率 80.2%

反応条件

温度: 80 °C

実験手順

The mixture of 4-chloro-3-(trifluoromethyl)phenol (7.61 g, 38.7 mmol), 3,4-difluorobenzaldehyde (5.0 g, 35.2 mmol) and CS2CO3 (11.46 g, 35.2 mmol) was heated with a microwave reactor at 80° C. for 1 h. Purification via a flash column chromatography then afforded the title compound (9.0 g, 80% yield). LCMS: rt=3.80 min, [M+H+]=319

後処理

customPurification via a flash column chromatography

出典と根拠

ORDレコード: ord-21434702cf90401aa990593e126efa84
出典データセット: uspto-grants-2014_01
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08637536B2

反応ノート

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