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Potassium Bromide → Methyl 2-bromo-2-(3,5-dichlorophenyl)acetate

HRID 1666300
ノート
印刷プレビュー

反応式

HRID 1666300 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9](OS(C)(=O)=O)[C:10]([O:12][CH3:13])=[O:11])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[Br-:19].[K+]>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]([Br:19])[C:10]([O:12][CH3:13])=[O:11])[CH:5]=[C:6]([Cl:8])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 253877Potassium BromideHCID 86629543HCID 86629543、化合物

生成物 1

HCID 77174840Methyl 2-bromo-2-(3,5-dichlorophenyl)acetate収率 102.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of methyl 2-(3,5-dichlorophenyl)-2-mesyloxyacetate (8.2 g) in dimethylformamide (30 ml) was treated with potassium bromide (4.0 g) at 50° C. for 1.5 hours. The reaction mixture was partitioned between water (200 ml) and ethyl acetate (300 ml). The organic phase was separated and washed twice with water (2×200 ml) and finally with saturated brine solution (200 ml). The ethyl acetate solution was dried and concentrated to dryness giving crude methyl 2-(3,5-dichlorophenyl)-2-bromoacetate (8 g). Filtration through a column of silica gel using dichloromethane as eluent gave the pure substance as an oil (7.4 g).

後処理

  1. customThe reaction mixture was partitioned between water (200 ml) and ethyl acetate (300 ml)
  2. customThe organic phase was separated
  3. washwashed twice with water (2×200 ml) and finally with saturated brine solution (200 ml)
  4. dry with materialThe ethyl acetate solution was dried
  5. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-602b5c95884249648066255bcff9c84b
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08044067B2

反応ノート

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