Methyl iodide → HCID 57742132, 화합물

HRID 660321노트

반응식

HRID 660321 반응식
[CH2:1]([O:3][C:4](=[O:16])[CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH2:13][O:14][CH3:15])[CH:7]=1)[CH3:2].[H-].[Na+].I[CH3:20]>CN(C=O)C>[CH2:1]([O:3][C:4](=[O:16])[CH:5]([C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH2:13][O:14][CH3:15])[CH:7]=1)[CH3:20])[CH3:2]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 57742154HCID 57742154, 화합물

생성물 1

HCID 57742132HCID 57742132, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a stirred solution of (3-Methoxymethoxy-phenyl)-acetic acid ethyl ester (31.2 g) in DMF (200 mL) was slowly added sodium hydride (6.21 g) and iodomethane (22.3 g) at 0°. After stirred for 20 h at 0°, this reaction mixture was quenched with water. This mixture was extracted with EtOAc, and combined organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo. The resulting residue was chromatographed on silica gel (n-Hex:EtOAc=10:1) to afford the product as colorless oil.

후처리

  1. customat 0°
  2. customthis reaction mixture was quenched with water
  3. extractionThis mixture was extracted with EtOAc
  4. dry with materialwas dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe resulting residue was chromatographed on silica gel (n-Hex:EtOAc=10:1)

출처 및 근거

ORD 기록
ord-7e16d92d5dfd4d97a3f2dd8ed40c00ae
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084484B2

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