Chloromethyl Methyl Ether → HCID 57742154, 화합물

HRID 660320노트

반응식

HRID 660320 반응식
[CH2:1]([O:3][C:4](=[O:13])[CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([OH:12])[CH:7]=1)[CH3:2].[H-].[Na+].[CH2:16](Cl)[O:17][CH3:18]>C1COCC1.O>[CH2:1]([O:3][C:4](=[O:13])[CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH2:16][O:17][CH3:18])[CH:7]=1)[CH3:2]

참가 물질

6

반응물 3

HCID 7864Chloromethyl Methyl EtherHCID 24758Sodium hydrideHCID 572437Ethyl (3-Hydroxyphenyl)acetate

생성물 1

HCID 57742154HCID 57742154, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (3-Hydroxy-phenyl)-acetic acid ethyl ester (27.6 g) in THF was added NaH (7.35 g), MOM-Cl (14.8 g) slowly at 0°. After stirred for 14 h at the same temperature, the reaction mixture was warmed to room temperature. The resulting mixture was diluted with water and extracted with EtOAc. The combined organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo. The resulting residue was chromatographed on silica gel (n-Hex:EtOAc=15:1 to 10:1) to afford the product as colorless oil. (31.2 g, 90.9%)

후처리

  1. extractionextracted with EtOAc
  2. dry with materialThe combined organic layer was dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe resulting residue was chromatographed on silica gel (n-Hex:EtOAc=15:1 to 10:1)

출처 및 근거

ORD 기록
ord-829b6dd1c705454b8688e0ae3af37fa8
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084484B2

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