1-(Bromomethyl)-2,3-difluoro-benzene → Ethyl 2-(2,3-difluorobenzyl)-3-oxobutyrate

HRID 1674156ノート

反応式

HRID 1674156 の反応式
Br[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([F:9])[C:4]=1[F:10].[Na].[C:12]([O:18][CH2:19][CH3:20])(=[O:17])[CH2:13][C:14]([CH3:16])=[O:15]>O1CCCC1>[F:10][C:4]1[C:5]([F:9])=[CH:6][CH:7]=[CH:8][C:3]=1[CH2:2][CH:13]([C:14](=[O:15])[CH3:16])[C:12]([O:18][CH2:19][CH3:20])=[O:17]

参加物

4

反応物 2

HCID 5179841-(Bromomethyl)-2,3-difluoro-benzeneHCID 87089461Ethyl acetoacetatesodium salt

生成物 1

HCID 57460769Ethyl 2-(2,3-difluorobenzyl)-3-oxobutyrate収率 79%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1-(bromomethyl)-2,3-difluorobenzene (1.6 g) and ethyl acetoacetate sodium salt (2.36 g) in tetrahydrofuran (20 mL) was stirred for 12 hr. The insoluble material was filtered off, and the filtrate was concentrated. The residue was purified by silica gel column chromatography to give the title compound (1.56 g, 79%) as a colorless viscous oil.

後処理

  1. filtrationThe insoluble material was filtered off
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-dc2356b681f2448abe1ec47d43d2b096
出典データセット
uspto-grants-2011_08
特許番号
US07998968B2

反応ノート

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