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Potassium Carbonate → HCID 53855288, 화합물

HRID 327980
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HRID 327980 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:18]=[CH:17][C:11]2[C:12](=[O:16])[CH2:13][CH2:14][O:15][C:10]=2[C:9]=1[CH2:19][CH2:20][CH3:21].[CH2:22]([O:24][C:25](=[O:46])[CH2:26][CH2:27][C:28]1[CH:33]=[C:32]([C:34]2[O:35][C:36](=[O:44])[C:37]3[CH:43]=[CH:42][CH:41]=[CH:40][C:38]=3[CH:39]=2)[CH:31]=[CH:30][C:29]=1[OH:45])[CH3:23].C(=O)([O-])[O-].[K+].[K+]>CC(=O)CC>[CH2:22]([O:24][C:25](=[O:46])[CH2:26][CH2:27][C:28]1[CH:33]=[C:32]([C:34]2[O:35][C:36](=[O:44])[C:37]3[CH:43]=[CH:42][CH:41]=[CH:40][C:38]=3[CH:39]=2)[CH:31]=[CH:30][C:29]=1[O:45][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:18]=[CH:17][C:11]2[C:12](=[O:16])[CH2:13][CH2:14][O:15][C:10]=2[C:9]=1[CH2:19][CH2:20][CH3:21])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 19921918HCID 19921918, 화합물HCID 54115240HCID 54115240, 화합물

생성물 1

HCID 53855288HCID 53855288, 화합물수율 58.1%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

A mixture of 0.352 g (0.99 mmol) of 7-[(5-bromopentyl)oxy]-2,3-dihydro-8-propyl-4H-1-benzopyran-4-one, 0.346 g (1.02 mmol) of 2-hydroxy-5-(1-oxo-1H-2-benzopyran-3-yl)benzenepropanoic acid ethyl ester, 0.574 g (4.15 mmol) of anhydrous granular potassium carbonate and 20.9 mL of 2-butanone was stirred and refluxed for 45 hrs. The resulting slurry was filtered with suction and the solids were washed thoroughly with ethyl acetate. The filtrate and washes were combined and concentrated in vacuo and the residue was purified by flash chromatography on 75 g of silica gel, eluting with 3:1 hexane-ethyl acetate, affording 0.352 g (58.1%) of the title compound as a white solid, mp 143.5°-144° C.

후처리

  1. temperaturerefluxed for 45 hrs
  2. filtrationThe resulting slurry was filtered with suction
  3. washthe solids were washed thoroughly with ethyl acetate
  4. concentrationconcentrated in vacuo
  5. customthe residue was purified by flash chromatography on 75 g of silica gel
  6. washeluting with 3:1 hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-570036ffa3554c929cf2de5f9f7239ce
출처 데이터셋
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05273999

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