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

HRID 536166

반응식

HRID 536166 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 24470Silver Nitrate촉매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-dc20eafd28f64893a4550c669ed52d48
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859573B2

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