Methyl iodide → (2-Chloro-6-fluoro-4-methoxyphenyl)methanol

HRID 1772875ノート

反応式

HRID 1772875 の反応式
CI.[Cl:3][C:4]1[CH:5]=[C:6]([OH:13])[CH:7]=[C:8]([F:12])[C:9]=1[CH2:10][OH:11].[C:14](=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:3][C:4]1[CH:5]=[C:6]([O:13][CH3:14])[CH:7]=[C:8]([F:12])[C:9]=1[CH2:10][OH:11]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 222200093-Chloro-5-fluoro-4-(hydroxymethyl)phenol

生成物 1

HCID 84771656(2-Chloro-6-fluoro-4-methoxyphenyl)methanol収率 100%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Methyl iodide (0.13 mL, 2.08 mmol) was added dropwise to a solution of 3-chloro-5-fluoro-4-(hydroxymethyl)phenol (334 mg, 1.89 mmol) and potassium carbonate (287 mg, 2.08 mmol) in DMF (5 mL) and the reaction mixture stirred for 4 h at rt. The reaction mixture was partitioned between DCM and H2O, the organic layer separated and the aqueous further extracted with DCM. The combined organic phases were concentrated in vacuo to yield the title compound as a yellow oil (360 mg, 1.89 mmol).

後処理

  1. customThe reaction mixture was partitioned between DCM and H2O
  2. customthe organic layer separated
  3. extractionthe aqueous further extracted with DCM
  4. concentrationThe combined organic phases were concentrated in vacuo

出典と根拠

ORDレコード
ord-bc9740bfbae847569450f1f5e71b7003
出典データセット
uspto-grants-2016_02
特許番号
US09249160B2

反応ノート

読み込み中…