Water → HCID 57742154, 화합물

HRID 660308노트

반응식

HRID 660308 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[CH:6][CH:7]=1.[H-].[Na+].Cl[CH2:17][O:18][CH3:19].O>C1COCC1>[CH3:17][O:18][CH2:19][O:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 7864Chloromethyl Methyl EtherHCID 24758Sodium hydrideHCID 572437Ethyl (3-Hydroxyphenyl)acetate

생성물 1

HCID 57742154HCID 57742154, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl 2-(3-hydroxyphenyl)acetate (24 g, 80.51 mmol) in THF (100 mL) was slowly added sodium hydride (2.93 g, 73.3 mmol) and chloromethylmethylether (5.94 g, 73.7 mmol) at 0° C. The reaction mixture was stirred for 16 hours at room temperature. The mixture was added water (200 mL) and extracted with EtOAc. The organic layer was dried with MgSO4. The organic layer was filtered and the filtrate was concentrated in vacuo. The residue was purified by column chromatography eluting with n-Hexane/EtOAc=10/1.

후처리

  1. customat 0° C
  2. extractionextracted with EtOAc
  3. dry with materialThe organic layer was dried with MgSO4
  4. filtrationThe organic layer was filtered
  5. concentrationthe filtrate was concentrated in vacuo
  6. customThe residue was purified by column chromatography
  7. washeluting with n-Hexane/EtOAc=10/1

출처 및 근거

ORD 기록
ord-21179bb2e1e7436489c4de8b8706901a
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084484B2

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