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Potassium Carbonate → HCID 59418747, 화합물

HRID 1896606
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HRID 1896606 반응식
CC1(C)C(C)(C)OB([C:9]2[CH:18]=[C:17]3[C:12]([CH2:13][CH2:14][CH2:15][NH:16]3)=[CH:11][CH:10]=2)O1.[CH2:20]([O:27][C:28]1[C:29]([C:35]([O:37][CH3:38])=[O:36])=[N:30][C:31](Br)=[CH:32][CH:33]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C([O-])([O-])=O.[K+].[K+].O1CCOCC1>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.O>[CH2:20]([O:27][C:28]1[C:29]([C:35]([O:37][CH3:38])=[O:36])=[N:30][C:31]([C:9]2[CH:18]=[C:17]3[C:12]([CH2:13][CH2:14][CH2:15][NH:16]3)=[CH:11][CH:10]=2)=[CH:32][CH:33]=1)[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1
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참가 물질

8

반응물 4

HCID 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 59418684Methyl 3-(benzyloxy)-6-bromopicolinateHCID 594187157-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,3,4-tetrahydroquinoline

생성물 1

HCID 59418747HCID 59418747, 화합물

시약·촉매·용매 3

HCID 74236
Tetrabutylammonium Bromide
촉매
HCID 178418476HCID 178418476, 화합물촉매
HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

To 7-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1,2,3,4-tetrahydroquinoline (27B) (1.16 g, 4.48 mmol), methyl 3-(benzyloxy)-6-bromopicolinate (29A) (1.44 g, 4.48 mmol), K2CO3 (1.546 g, 11.2 mmol), tetrabutylammonium bromide (0.144 g, 0.45 mmol), and dichlorobis(triphenylphosphine)palladium(II) (126 mg, 0.18 mmol) was added 1,4-dioxane (30 mL) and water (15 mL). The reaction mixture was heated to 90° C. for 1.5 hours, cooled to rt, concentrated, diluted with EtOAc, washed sequentially with water, brine, dried over MgSO4, filtered, and concentrated under reduced pressure. The crude material was precipitated from EtOAc/PE to provide the product methyl 3-(benzyloxy)-6-(1,2,3,4-tetrahydroquinolin-7-yl)picolinate (29B). Additional material was isolated from the filtrate by column chromatography on silica gel eluting with a gradient of PE:EtOAc 73:27-63:37, to provide the desired product (29B): 1H NMR (300 MHz, CDCl3) δ 7.67 (1H, d), 7.48-7.44 (2H, m), 7.43-7.31 (4H, m), 7.21 (1H, d), 7.16 (1H, dd), 7.01 (1H, d) 5.21 (2H, s), 3.98 (3H, s), 3.34 (2H, m), 2.79 (2H, t), 1.96 (2H, m).

후처리

  1. temperaturecooled to rt
  2. concentrationconcentrated
  3. additiondiluted with EtOAc
  4. washwashed sequentially with water, brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe crude material was precipitated from EtOAc/PE

출처 및 근거

ORD 기록
ord-f882282d1c9d4ed4b98de1840f7c5c8e
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08518970B2

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