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Sulfuric Acid → HCID 15295001, 화합물

HRID 327944
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HRID 327944 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].C([O:24][C:25]([C:27]1[O:28][C:29]2[C:35]([OH:36])=[CH:34][CH:33]=[CH:32][C:30]=2[CH:31]=1)=[O:26])C.C(=O)([O-])[O-].[K+].[K+].O.[OH-].[Li+].S(=O)(=O)(O)O>C1COCC1.O.C(OCC)(=O)C.CCOCC.CC(=O)CC>[O:16]=[C:12]1[C:11]2[CH:17]=[CH:18][C:8]([O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][O:36][C:35]3[C:29]4[O:28][C:27]([C:25]([OH:26])=[O:24])=[CH:31][C:30]=4[CH:32]=[CH:33][CH:34]=3)=[C:9]([CH2:19][CH2:20][CH3:21])[C:10]=2[O:15][CH2:14][CH2:13]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 5

HCID 1118Sulfuric AcidHCID 11430Potassium CarbonateHCID 168937Lithium hydroxide, monohydrateHCID 19921918HCID 19921918, 화합물HCID 21400703Ethyl 7-hydroxy-1-benzofuran-2-carboxylate

생성물 1

HCID 15295001HCID 15295001, 화합물수율 74.9%

시약·촉매·용매

5
HCID 962Water용매HCID 3283Diethyl Ether용매HCID 6569Methyl Ethyl Ketone용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 0.556 g (1.57 mmol) of 7-[(5-bromopentyl)oxy]-2,3-dihydro-8-propyl-4H-1-benzopyran-4-one, 0.323 g (1.57 mmol) of 7-hydroxy-2-benzofurancarboxylic acid ethyl ester, 0.866 g (6.26 mmol) of anhydrous granular potassium carbonate and 16 mL of 2-butanone was stirred and refluxed for 16.5 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 70 g of silica gel, eluting with 4:1 hexane-ethyl acetate giving 0.527 g (70%) of 7-[5-[(3,4-dihydro-4-oxo-8-propyl-2H-1-benzopyran-7-yl)oxy]pentyloxy]benzenepropanoic acid ethyl ester as a white solid, mp 79.5°-81° C. A mixture of 0.262 g (0.55 mmol) of this ester in 3.5 mL of THF and 3.5 mL of water was treated with 35.1 mg (0.84 mmol) of lithium hydroxide monohydrate and the mixture was stirred for 17.5 hr. After being acidified with 16 mL of 3N aqueous sulfuric acid, the resulting mixture was worked-up with ether and ethyl acetate in the usual manner. The crude product was recrystallized from hexane-ethyl acetate to give 0.185 g (74.9%) of the title compound as a white solid, mp 152°-153.5° C.

후처리

  1. temperaturerefluxed for 16.5 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 70 g of silica gel
  6. washeluting with 4:1 hexane-ethyl acetate giving 0.527 g (70%) of 7-[5-[(3,4-dihydro-4-oxo-8-propyl-2H-1-benzopyran-7-yl)oxy]pentyloxy]benzenepropanoic acid ethyl ester as a white solid, mp 79.5°-81° C
  7. stirringthe mixture was stirred for 17.5 hr
  8. customThe crude product was recrystallized from hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-9d69c55117a2426da35c84b996250309
출처 데이터셋
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05273999

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