Potassium Carbonate → 2-Benzyloxy-5-methoxy-benzaldehyde

HRID 1096678

반응식

HRID 1096678 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:3]=1[CH:4]=[O:5].F[C:13]1[CH:20]=[CH:19][C:16]([CH2:17]Br)=[CH:15][CH:14]=1.C([O-])([O-])=O.[K+].[K+]>CC#N>[CH2:17]([O:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:3]=1[CH:4]=[O:5])[C:16]1[CH:19]=[CH:20][CH:13]=[CH:14][CH:15]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 680214-Fluorobenzyl bromideHCID 956952-Hydroxy-5-methoxybenzaldehyde

생성물 1

HCID 8784742-Benzyloxy-5-methoxy-benzaldehyde수율 88%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 2-hydroxy-5-methoxybenzaldehyde (0.152 g, 1.0 mmol) in dry MeCN (50 mL) was added 4-fluorobenzyl bromide (0.145 mg, 1.0 mmol), and anhydrous K2CO3 (0.27 g, 2.0 mmol). The mixture was refluxed under stirring for 4 h, and then evaporated in vacuo. Water (100 mL) was added and the mixture was extracted with EtOAc. The separated organic layer was dried with MgSO4, and then evaporated in vacuum. Finally, the residue was eluted through a silica gel column with n-hexane/EtOAc (4:1) to give white compound I (0.21 g, 88%).

후처리

  1. temperatureThe mixture was refluxed
  2. customevaporated in vacuo
  3. additionWater (100 mL) was added
  4. extractionthe mixture was extracted with EtOAc
  5. dry with materialThe separated organic layer was dried with MgSO4
  6. customevaporated in vacuum
  7. washFinally, the residue was eluted through a silica gel column with n-hexane/EtOAc (4:1)

출처 및 근거

ORD 기록
ord-bb68b901dcb44636822a38820b58eafb
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08138360B2

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