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Potassium Carbonate → 1-(2,3-Dihydropyrano[4,3,2-de]quinolin-7-yl)-3-methylnaphthalen-2-ol

HRID 514005
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HRID 514005 반응식
Br[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[C:4]([CH3:12])[C:3]=1[OH:13].OC(C(F)(F)F)=O.[O:21]1[C:32]2[C:33]3[C:28]([C:29](B(O)O)=[CH:30][CH:31]=2)=[N:27][CH:26]=[CH:25][C:24]=3[CH2:23][CH2:22]1.C([O-])([O-])=O.[K+].[K+].CC(N(C)C)=O>C(OCC)(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O>[O:21]1[C:32]2[C:33]3[C:28]([C:29]([C:2]4[C:11]5[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=5)[CH:5]=[C:4]([CH3:12])[C:3]=4[OH:13])=[CH:30][CH:31]=2)=[N:27][CH:26]=[CH:25][C:24]=3[CH2:23][CH2:22]1
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반응물 4

HCID 11430Potassium CarbonateHCID 31374DimethylacetamideHCID 671260591-Bromo-3-methylnaphthalen-2-olHCID 1317332892,3-dihydropyrano[4,3,2-de]quinolin-7-ylboronic acid TFA salt

생성물 1

HCID 671260371-(2,3-Dihydropyrano[4,3,2-de]quinolin-7-yl)-3-methylnaphthalen-2-ol수율 29.1%

시약·촉매·용매 3

HCID 178418397
HCID 178418397, 화합물
촉매
HCID 962Water용매
HCID 8857Ethyl Acetate용매

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온도
110 °C

실험 절차

1-Bromo-3-methylnaphthalen-2-ol (5B) (340 mg, 1.43 mmol), 2,3-dihydropyrano[4,3,2-de]quinolin-7-ylboronic acid TFA salt (5C) (566 mg, 1.72 mmol), Pd(PPh3)4 (166 mg, 0.14 mmol) and K2CO3 (991 mg, 7.15 mmol) were added to a degassed solution of DMA (6 mL) and water (2 mL) and heated to 110° C. in a microwave for 1 h. The reaction mixture was cooled, diluted with ethyl acetate and washed with saturated sodium bicarbonate solution, brine and dried (MgSO4), filtered, concentrated and purified by flash column chromatography (silica gel, ethyl acetate/hexanes) to give 5D (136 mg, 29%). LCMS-ESf+ (m/z): [M+H]+ calcd for C22H18NO2: 328.38. Found: 328.2.

후처리

  1. temperatureThe reaction mixture was cooled
  2. washwashed with saturated sodium bicarbonate solution, brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. custompurified by flash column chromatography (silica gel, ethyl acetate/hexanes)

출처 및 근거

ORD 기록
ord-c8aee430d6b14871b4531e891e8a4ad9
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09102614B2

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