Acetone → HCID 66611398, 화합물

HRID 330835노트

반응식

HRID 330835 반응식
Br[CH2:2][CH2:3][CH3:4].C([O-])([O-])=O.[K+].[K+].CC(C)=O.[CH3:15][O:16][C:17](=[O:26])[C:18]1[CH:23]=[C:22]([OH:24])[CH:21]=[CH:20][C:19]=1[I:25]>O>[CH3:15][O:16][C:17](=[O:26])[C:18]1[CH:23]=[C:22]([O:24][CH2:2][CH2:3][CH3:4])[CH:21]=[CH:20][C:19]=1[I:25]

참가 물질

6

반응물 4

HCID 180AcetoneHCID 78401-Bromopropane2회HCID 11430Potassium Carbonate2회HCID 22349232Methyl 5-hydroxy-2-iodobenzoate

생성물 1

HCID 66611398HCID 66611398, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2.97 mL (32.7 mmol) 1-bromopropane and 299 mg (1.80 mmol) KI are added to a mixture of 3.39 g (24.5 mmol) K2CO3 and 200 mL acetone. The mixture is stirred for 30 min at reflux. Subsequently, 5.00 g (18.0 mmol) methyl-5-hydroxy-2-iodobenzoate are added and the resulting mixture is refluxed for 2 h. One additional equivalent of 1-bromopropane and of K2CO3 is added and refluxing is continued for 12 h. Water is added and the mixture is extracted with EtOAc. The organic layer is dried over sodium sulphate and the solvent is removed in vacuo. The crude product is purified by column chromatography (silica gel, heptane/EtOAc 100/0→60/40). The product is used without further characterization.

후처리

  1. temperatureat reflux
  2. temperaturethe resulting mixture is refluxed for 2 h
  3. temperaturerefluxing
  4. waitis continued for 12 h
  5. extractionthe mixture is extracted with EtOAc
  6. dry with materialThe organic layer is dried over sodium sulphate
  7. customthe solvent is removed in vacuo
  8. customThe crude product is purified by column chromatography (silica gel, heptane/EtOAc 100/0→60/40)

출처 및 근거

ORD 기록
ord-96c57ac3370d49e88fa044fe82c12f16
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877754B2

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