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

HRID 1772875노트

반응식

HRID 1772875 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-bc9740bfbae847569450f1f5e71b7003
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09249160B2

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