Ethanol → 6-Chloro-5-fluoropyridine-3-carbaldehyde

HRID 536166

反応式

HRID 536166 の反応式
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([CH:9](Br)Br)=[CH:4][N:3]=1.C([OH:14])C>[N+]([O-])([O-])=O.[Ag+].O>[Cl:1][C:2]1[N:3]=[CH:4][C:5]([CH:9]=[O:14])=[CH:6][C:7]=1[F:8]

参加物

5

反応物 2

HCID 702EthanolHCID 866970262-Chloro-5-(dibromomethyl)-3-fluoropyridine

生成物 1

HCID 216981946-Chloro-5-fluoropyridine-3-carbaldehyde

試薬・触媒・溶媒 2

HCID 24470Silver Nitrate触媒HCID 962Water溶媒

実験手順

A suspension 2-chloro-5-(dibromomethyl)-3-fluoropyridine (2.3 g, 7.58 mmol), silver nitrate (5.15 g, 30.3 mmol) in a mixed solvents of ethanol (10 mL) and water (10 mL) was stirred for 1 h at 100° C., then filtrated, and concentrated. The residue was dissolved in ethyl acetate, washed with water and brine, dried over sodium sulfate, concentrated. Purification via ISCO system afforded the title product (1.0 g) as a pale solid. LC-MS (ESI): m/z 159 [M+H]+; 2.01 min (ret time).

後処理

  1. filtrationfiltrated
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water and brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customPurification via ISCO system

出典と根拠

ORDレコード
ord-dc20eafd28f64893a4550c669ed52d48
出典データセット
uspto-grants-2014_10
特許番号
US08859573B2

関連ノート

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