Potassium Carbonate → HCID 58951921, 화합물

HRID 1694793

반응식

HRID 1694793 반응식
[OH:1][C:2]1[C:9]([CH:10]=O)=[CH:8][C:7]([CH3:12])=[CH:6][C:3]=1[CH:4]=[O:5].C(=O)([O-])[O-].[K+].[K+].Br[CH:20](C(OCC)=O)[C:21]([O:23][CH2:24][CH3:25])=[O:22]>CN(C=O)C>[CH2:24]([O:23][C:21]([C:20]1[O:1][C:2]2[C:3]([CH:4]=[O:5])=[CH:6][C:7]([CH3:12])=[CH:8][C:9]=2[CH:10]=1)=[O:22])[CH3:25]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 69637Diethyl bromomalonateHCID 817442,6-Diformyl-4-methylphenol

생성물 1

HCID 58951921HCID 58951921, 화합물수율 94.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

A solution of 2-hydroxy-5-methylisophtalaldehyde (1 g) in DMF (10 ml) was treated under an Argon atmorphere with potassium carbonate (1.01 g) and diethyl bromomalonate (1.60 g). The reaction mixture was heated to 100° C. for 20 hrs, then cooled to r.t., quenched with water and extracted with EtOAc. The organics were dried over MgSO4, filtrated and concentrated to obtain 7-formyl-5-methyl-benzofuran-2-carboxylic acid ethyl ester (1.34 g) as off-white solid. MS (ISP): 233.1 ((M+H)+.). The crude product was used in the next reaction step without further purification.

후처리

  1. temperaturecooled to r.t.
  2. customquenched with water
  3. extractionextracted with EtOAc
  4. dry with materialThe organics were dried over MgSO4
  5. filtrationfiltrated
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-58a6c1d77a5a4d58bdb1ebdd7c541ccf
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158668B2

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